Month: February 2021

1000994-95-5, name is 1-Bromo-4-(1,1-difluoroethyl)benzene, belongs to bromides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: 1000994-95-5

Nitrogen,Titration in the following -60 1.6M n-butyllithium in hexane (0.4 mL)in1-Bromo-4- (1,1-difluoroethyl) benzene(0.17 g)Of tetrahydrofuran (0.61 g)The solution was stirred for an additional 1 hour and titrated for 4 minutes5-cyclopropyl-6-methoxymethylpyridinecarbonitrile(0.10 g)In tetrahydrofuran (0.30 g).After stirring for 2 hours and 2 minutes, the temperature was further raised to room temperature.After adding 5% aqueous hydrochloric acid solution (0.93 g) and stirring,Water and ethyl acetate were added,The mixture was separated into a mixture of an organic layer and an aqueous layer.Ethyl acetate (4 mL) was added to the resulting aqueous layer,Mixed and separated into an organic layer and an aqueous layer.Mixing the organic layers of both,The mixture was separated by adding 5% aqueous sodium hydrogencarbonate solution, and the organic layer and the aqueous layer were mixed.Ethyl acetate (2 mL) was added to the resulting aqueous layer,Mixed and separated into an organic layer and an aqueous layer.The organic layers were mixed, and the organic layer and the aqueous layer were mixed by adding water. Ethyl acetate (2 mL) was added to the obtained aqueous layer, mixed, and separated into an organic layer and an aqueous layer. The organic layers were mixed, dried by addition of sodium sulfate, and after the desiccant was filtered off, the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane / ethyl acetate = 49/1, v / v)To obtain the title compound (0.14 g, yield 75.1%) as a pale yellow oily substance.

The synthetic route of 1000994-95-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NISSAN CHEMICAL INDUSTRIES, LTD.; YOSHINO, HIRONOBU; UMEDA, YASUHIRO; TAKEOKA, JUN; NAGAYA, AKIHIRO; SUGAWARA, YUDAI; YOSHINO, MADOKA; (54 pag.)TW2016/5826; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 67344-77-8, name is 1-(3-Bromophenyl)-N-methylmethanamine, A new synthetic method of this compound is introduced below., Computed Properties of C8H10BrN

To a solution of compound 14 (23.1 g, 115.5 mmol) in methylene chloride (500 mL) was added alpha-bromo-2?-acetonapthone (27.9 g, 110.0 mmol) and the resulting mixture was stirred at 0¡ã C. for 1 h prior to the addition of triethylamine (15.3 mL, 47.4 mmol). The reaction mixture was stirred at 0¡ã C. for 2 h. The resulting mixture was diluted with water (200 mL) and the aqueous phase was extracted with additional methylene chloride (2¡Á200 mL). The combined extracts were dried over sodium sulfate, filtered and concentrated to afford compound 15 (44.5 g) as a light yellow oil, which was used in the next step without further purification: 1H NMR (CDCl3, 500 MHz) 8.49 (s, 1H), 8.01 (dd, J=8.8, 1.8 Hz, 1H), 7.95 (d, J=8.0 Hz, 1H), 7.90-7.84 (m, 2H), 7.62-7.52 (m, 3H), 7.40 (d, J=8.0 Hz, 1H), 7.31 (d, J=8.0 Hz, 1H), 7.19 (t, J=7.7 Hz, 1H), 3.91 (s, 2H), 3.68 (s, 2H), 2.40 (s, 3H)

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Qiu, Jun; Gao, Qui; Liu, Shuang; Hu, Min; Yang, Yuh-Lin Allen; Isherwood, Matthew; Amin, Rasidul; US2014/275101; (2014); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 626-88-0,Some common heterocyclic compound, 626-88-0, name is 1-Bromo-4-methylpentane, molecular formula is C6H13Br, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Step 1: 2-(4-methylpentyl)-1H-isoindole-1,3(2H)-dione To a solution of 1-bromo-4-methylpentane (5.0 g, 0.030 mol) in DMF (20 mL) was added potassium phthalimide (5.9 g, 0.032 mol) in one portion at room temperature. After stirring at room temperature of 1 hr, the mixture was heated at 55 C. for 16 hr. Chloroform (30 mL) was added to the reaction mixture and the resulting mixture was poured into water (100 mL). The aqueous phase was extracted with chloroform and the combined organic phase was washed with 0.25 M NaOH (aq) and water. The organic phase was dried (Na2SO4), filtered and concentrated in vacuo to give 2-(4-methylpentyl)-1H-isoindole-1,3(2H)-dione as a pale yellow oil. (M+H) 232, 2.80 min. (LC/MS method A).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-4-methylpentane, its application will become more common.

Reference:
Patent; IGNAR, DIANE MICHELE; US2010/113512; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 2862-39-7, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 2862-39-7, name is 2-Bromo-N,N-dimethylethanamine hydrobromide belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a stirred solution of 6-(4-chlorophenyl)-5-(3, 8-dimethyl-[1 ,2,4]triazolo[4, 3-a]pyridin-6-yl)-3-methyl-5,6-dihydropyrrolo[3,4-b]pyrrol-4(1H)-one (Step 10 of Example 3, 100 mg, 0.255 mmol)in DMF (4 mL) was added NaH (13.27 mg, 0.332 mmol) under Ar. After 30 mm at rt, 3-bromo-1- methypyrrolidin-2-one (54.5 mg, 0.306 mmol) was added. The reaction mixture stirred for 1 h at rt, quenched with a saturated aqueous solution of NaHCO3 (75 mL) and extracted with EtOAc (2 x 75 mL). The organic layers were combined, washed with a saturated aqueous solution of NaHCO3 (75 mL), dried on Na2504 and evaporated. The residue was purified by silica gelchromatography on Combiflash Isco (eluent: DCM/MeOH; gradient: 0-10% MeOH in 12 mm, 2 mm 10% MeOH; flow: 18 mL/min) and subsequent SF0 to afford 12 mg of diastereomerA and 25 mg of diastereomer B. The title compound was prepared using an analogous procedure to that described in Example 126 but using dimethylaminoethyl bromide hydrobromide (71.3 mg, 0.306 mmol, 1.2 eq) and 3eq of NaH. The crude product was purified by silica gel chromatography on Combiflash Isco (eluent: DCM/MeOH; gradient: 0-10% MeOH in 12 mm, 3.6 mm 10% MeOH; flow: 18 mL/min) and subsequent trituration of the resulting material in diethyl ether to afford (65 mg) of the title compound as a colorless solid. Rt: 0.62 mm (LC-MS 1); ESI-MS mlz: 463.2 [M+H] (LC-MS 1); 1H NMR (400 MHz, DMSO-d6) O 8.31 (d, J = 1.7 Hz, 1H), 7.42- 7.26 (m, 5H), 6.71 (5, 1H), 6.42(5, 1H), 3.72-3.57 (m, 1H), 3.57-3.44 (m, 1H), 2.59 (5, 3H), 2.41 (5, 3H), 2.29-2.18 (m, 1H),2.14 (5, 3H), 2.08- 1.91 (m, 7H).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-Bromo-N,N-dimethylethanamine hydrobromide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NOVARTIS AG; BLANK, Jutta; BOLD, Guido; BORDAS, Vincent; COTESTA, Simona; GUAGNANO, Vito; RUeEGER, Heinrich; VAUPEL, Andrea; WO2015/75665; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 1647-26-3, name is 1-Bromo-2-cyclohexylethane, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 1647-26-3

1-(2-Chloro-phenyl)-3-cyclohexyl-propan-1-one 15.57 g (640 mmole) Magnesium turnings were placed in a 1 l-roundbottom flask equipped with a dropping funnel and a reflux condenser, and 50 ml of THF were added. The magnesium was etched slightly with a few crystals of iodine and then 2 g of (2-bromo-ethyl)-cyclohexane were added and the mixture was heated locally. After the start of the Grignard-formation the rest of the (2-bromo-ethyl)-cyclohexane in 350 ml of THF (112.65 g in total, 589 mmole) were added within a period of 20 min. The mixture was refluxed for 1.5 h and then cooled to room temperature. In a separate 2 l-roundbottom flask 70.5 g (513 mmole) of 2-chloro-benzonitrile and 156 mg (0.16 mole %) copper(I)iodide were dissolved in 130 ml of THF. The Grignard-solution was added dropwise over a period of 30 min and the reaction mixture was refluxed for 3 h. After standing overnight at room temperature, a mixture of 190 ml water and 127 ml concentrated hydrochloric acid were added very carefully, causing a strongly exothermic reaction. The mixture was stirred at 50 C. for 1 h and the layers were separated. The aqueous layer was extracted twice with 150 ml of toluene each. The combined organic layers were washed twice with 2 M sulphuric acid, once with a saturated sodium bicarbonate solution and once with a saturated sodium chloride solution. After drying over magnesium sulphate the solvent was evaporated in vacuo to yield 133.5 g (quant.) of the desired phenone as slightly brown oil. 1H-NMR (400 MHz, CDCl3): delta=7.41-7.14 (m, 4H, aromatic), 2.91 (t, 2H, COCH2), 1.71-1.55, 1.28-1.10, 0.93-0.85 (3*m, 13H) ppm.

According to the analysis of related databases, 1647-26-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Lammus Novolen Technology GmbH; US8299287; (2012); B2;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 129316-09-2, A common heterocyclic compound, 129316-09-2, name is 1,3-Dibromo-5-(tert-butyl)benzene, molecular formula is C10H12Br2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Step 1 : 1-(3-Bromo-5-(terf-butyl)phenyl)cvclobutanol (P23a) To an oven dried 100 mL 3-neck flask was added 1 ,3-dibromo-5-(terf-butyl)benzene (500 mg, 1.72 mmol) in dry THF (30 mL) under N2 and the mixture was cooled to -78C. n-BuLi (2.5M, 1 mL) was added and the mixture was stirred at -78C for 1 h. Then cyclobutanone (181 mg, 2.58 mmol) was added. After the reaction was complete (monitored by LC-MS) the mixture was quenched with aq. NH4CI and extracted with EA. The organic layer was dried over MgS04, filtered and evaporated to give compound P23a (243 mg, 50%) as a yellow solid.

The synthetic route of 129316-09-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PHENEX PHARMACEUTICALS AG; STEENECK, Christoph; KINZEL, Olaf; GEGE, Christian; KLEYMANN, Gerald; HOFFMANN, Thomas; WO2013/79223; (2013); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 452-63-1, name is 1-Bromo-4-fluoro-2-methylbenzene, A new synthetic method of this compound is introduced below., name: 1-Bromo-4-fluoro-2-methylbenzene

Step 1: A mixture of 2-bromo-5-fluorotoluene (2.0 g, 11 mmol), acrylamide (1.5 g, 21 mmol), P(o-tolyl)3 (320 mg, 1.1 mmol), and Et3N (2.9 mL, 21 mmol), in toluene (25 mL) was deoxygenated by bubbling a stream of Ar through the solution for 15 minutes. Palladium(II) acetate (120 mg, 0.53 mmol) was added to the reaction mixture, and a stream of Ar was again passed through the mixture for 15 minutes. The reaction was heated to 140 C. for 2.25 hours, then cooled to ambient temperature, diluted with EtOAc, and filtered through Celite. The filtrate was washed with H2O, 1N HCl, H2O, dried (Na2SO4), filtered, and concentrated under reduced pressure to give amide 78 (1.7 g, 86%) which was used without further purification: 1H NMR (500 MHz, DMSO-d6): ?7.60-7.52 (m, 3H), 7.15-7.04 (m, 3H), 6.46 (d, J=16 Hz, 1H), 2.37 (s, 3H).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Nikam, Sham Shridhar; Scott, Ian Leslie; Sherer, Brian Alan; Wise, Lawrence David; US2003/236252; (2003); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 3017-70-7,Some common heterocyclic compound, 3017-70-7, name is 2-Bromo-3-methyl-2-butene, molecular formula is C5H9Br, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

[00329] In a reaction tube under nitrogen, a mixture of PdCl2(dppf)CH2Cl2 (22 mg; 0.027 mmol) and triethylamine (0.36 ml; 2.58 mmol) in dioxane (4 ml; dried over 4 ? sieves) was sealed and stirred at 80 C. overnight (18 h). After cooling to room temperature, 1.29M HB(pin) in dioxane (1.00 ml; 1.29 mmol) and 2-bromo-3-methyl-2-butene (131 mg; 0.879 mmol) were added and the reaction mixture was stirred at 80 C. GC analysis after 24 hours showed a new peak at 5.0 minutes which was identified by GC/MS as the desired borate compound.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Bromo-3-methyl-2-butene, its application will become more common.

Reference:
Patent; Commonwealth Scientific and Industrial Research Organisation; US6680401; (2004); B1;,
Bromide – Wikipedia,
bromide – Wiktionary

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 586-77-6, name is 4-Bromo-N,N-dimethylaniline, This compound has unique chemical properties. The synthetic route is as follows., Safety of 4-Bromo-N,N-dimethylaniline

General procedure: A round-bottom flask was chargedwith N,N-dialkyl aniline dissolved in toluene solution, under N2 condition. TBHP was added drop wise and reaction was stirred for 2 min. Triethylamine was added thereafter, and then the contents of the reaction were stirred for 3 h at 110 C under inert N2 condition. The reaction mixture was washed 2-3 times with H2O and ethyl acetate. The upper organic layer was separated and dried over sodium sulphate and then subjected to rotavapour. The crude mixture was purified by column chromatography on silica gel (60-120).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 586-77-6.

Reference:
Article; Botla, Vinayak; Barreddi, Chiranjeevi; Daggupati, Ramana V; Malapaka, Chandrasekharam; Journal of Chemical Sciences; vol. 128; 9; (2016); p. 1469 – 1473;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 445-02-3, A common heterocyclic compound, 445-02-3, name is 4-Bromo-2-(trifluoromethyl)aniline, molecular formula is C7H5BrF3N, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

To a mixture of 2-amino-5-bromobenzotrifluoride (1.0 g, 4.17 mmol) in DCM (10 mL) at 0-5C was added NEt3 (1.16 mL, 8.33 mmol), then methanesulfonyl chloride (0.389 mL, 5 mmol) dropwise. The reaction mixture was stirred at rt for 4 days. After 2 days, more NEt3 was added (1.16 mL, 8.33 mmol). As there was no evolution after 3 days, more NEt3 (0.580 mL, 4.17 mmol) and methanesulfonyl chloride (0.324 mL, 4.17 mmol) were added. The reaction was not completed, so the reaction mixture was then heated in a microwave oven at 1 10C for 20 min. There was no evolution, so the reaction was stopped. The reaction mixture was diluted with water and DCM. Layers were separated. The organic layer was washed with water, dried over MgS04 and evaporated. Purification by Flash chromatography using CombiFlash Companion ISCO system (Redisep silica 40g column, eluting with Cyclohexane/EtOAc 100:0 to 70:30) did not give the pure compound. Purification by prep HPLC using Gilson system (SunFire C18 column, eluting with H20 + 0.1 % TFA / CH3CN 20% to 85%) gave the title compound (404 mg, 31 % yield) as a white solid. 1H-NMR (400 MHz, DMSO-de, 298 K): delta ppm 3.12 (s, 3H) 7.55 (d, 1 H) 7.91 (d, 1 H) 7.92 (s, 1 H) 9.56 (s, 1 H). MS(10): 316.3-318.2 [M-1 ]

The synthetic route of 445-02-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; COOKE, Nigel Graham; FERNANDES GOMES DOS SANTOS, Paulo Antonio; FURET, Pascal; HEBACH, Christina; HOeGENAUER, Klemens; HOLLINGWORTH, Gregory; KALIS, Christoph; LEWIS, Ian; SMITH, Alexander Baxter; SOLDERMANN, Nicolas; STAUFFER, Frederic; STRANG, Ross; STOWASSER, Frank; TUFILLI, Nicola; VON MATT, Anette; WOLF, Romain; ZECRI, Frederic; WO2013/88404; (2013); A1;,
Bromide – Wikipedia,
bromide – Wiktionary