Month: January 2021

Application of 2635-13-4, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 2635-13-4 as follows.

201mg (1mmol) of 3,4-methylenedioxybromobenzene, 1mL aqueous ammonia (25-28%, 13.3mmol), 8mg (0.1mmol) CuO, 79mg (0.2mmol) diethylenetriaminepentaacetic acid, 112mg ( 2mmol) KOH, 1mL H2O was added 10mL reaction tube, sealed and reacted at 100C for 12h. After the reaction was stopped, extraction with ethyl acetate, washed with brine, dried over anhydrous sodium sulfate, filtered, and the filtrate was evaporated under reduced pressure, purified by silica gel column chromatography purification, in 3,4-methylenedioxyaniline 100mg, The yield was 73%.

According to the analysis of related databases, 2635-13-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Sun Yat-Sen University; ZHU, XIN HAI; YANG, BO; LIAO, LI HAO; CENG, YONG HENG; WAN, YI QIAN; (9 pag.)CN103739417; (2016); B;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 4333-56-6, A common heterocyclic compound, 4333-56-6, name is Bromocyclopropane, molecular formula is C3H5Br, 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 stirred solution of 2-bromo-5-fluorophenol (1.0 g) in DMF (15 mL) in a microwave tube was added cesium carbonate (5.0 g), potassium iodide (130 mg) and bromocyclopropane (1.82 g). The mixture was heated in a microwave oven to 180 C for 1 h, to 200 C for 1 h and to 220 C for 1 h. Ethyl acetate was added and the mixture was washed with water. The organic phase was washed with saturated sodium chloride solution, dried (sodium sulfate) and the solvent was removed in vacuum. Silica gel chromatography gave 1.14 g of the title compound. 1H-NMR (300MHz, DMSO-d6): delta [ppm]= 0.62 – 0.88 (m, 4H), 3.90 – 4.00 (m, 1 H), 6.77 (td, 1 H), 7.23 (dd, 1 H), 7.48 – 7.63 (m, 1 H).

The synthetic route of 4333-56-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER INTELLECTUAL PROPERTY GMBH; BAYER PHARMA AKTIENGESELLSCHAFT; SCHULZE, Volker; KOSEMUND, Dirk; WENGNER, Antje Margret; SIEMEISTER, Gerhard; STOeCKIGT, Detlef; BRUENING, Michael; WO2013/87579; (2013); 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. 67567-26-4, name is 4-Bromo-2,6-difluoroaniline, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 67567-26-4

Compound 121 : 4-(9-Cyclopentyl-7,7-difluoro-5-methyl-6-oxo-6,7,8,9- tetrahydro-5H-pyrimido[4,5-b][l,4]diazepin-2-ylamino)-3-fluoro-5-methoxybenzoic acid; [0581] 5-Bromo-l,3-difluoro-2-nitrobenzene: To a mixture of acetic acid (30 mL), 30% H2O2 (20 mL) and concentrated sulfuric acid (1 mL) was added l-bromo-2,6- difluoroaniline (5 g, 24 mmol) in acetic acid (10 mL) dropwise at 85 0C. The reaction mixture was heated for 1 h. It was then cooled down, diluted to water and extracted with ethyl acetate. The organic layer was dried and concentrated to a red residue, which was purified by flash column (EtOAc in Hexane 2-5%) to give the product as yellow solid (2.7 g, 47%). 1H NMR (400 MHz, CHLOROFORM-J) delta ppm 7.33 (m, 2 H).

According to the analysis of related databases, 67567-26-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; WO2009/42711; (2009); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 142808-15-9, name is 4-Bromo-2-fluorobenzotrifluoride, 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. Recommanded Product: 142808-15-9

To a reaction vessel under a nitrogen atmosphere, 4-bromo-2-fluoro-1-(trifluoromethyl)benzene (2.28 g) and diethyl ether (70 ml) were added, and cooling was carried out to-70C. Thereto, a n-butyllithium (1.57 M) n-hexane solution (7.10 ml) was added dropwise in a temperature range of -70C to -65C, and stirring was carried out for another 1 hour. Subsequently, a diethyl ether (10 ml) solution of compound (T-9) (2.68 g) was added dropwise in a temperature range of -70C to -65C, and stirring was carried out for 4 hours while returning to room temperature. The resultant reaction mixture was poured into ice water (100 ml), and mixing was carried out. Toluene (100 ml) was added to separate layers into an organic layer and an aqueous layer, and an extraction operation was performed. The resultant organic layer was sequentially washed with a 1 N hydrochloric acid solution, a saturated aqueous solution of sodium hydrogencarbonate and water, and drying over anhydrous magnesium sulfate was carried out. The resultant solution was concentrated under reduced pressure, and a residue was purified by fractionation by means of column chromatography (silica gel; heptane), and further purified by recrystallization from a heptane/Solmix A-11 mixed solvent, and thus (E)-1-(1,2-difluoro-2-[3-fluoro-4-(trifluoromethyl)phenyl]vinyl)-2 -fluoro-4-(4-propylcyclohexyl)benzene (1-1-25) (2.24 g) was obtained. The yield based on compound (T-9) was 57%. Chemical shifts according to 1H-NMR analysis were as described below, and the compound obtained could be identified to be (E)-1-(1,2-difluoro-2-[3-fluoro-4-(trifluoromethyl)phenyl]vinyl)-2 -fluoro-4-(4-propylcyclohexyl)benzene. Chemical shifts delta (ppm; CDCl3); 7.72 – 7.57 (m, 3H), 7.46 (dd, J = 7.65 Hz, J = 7.65 Hz, 1H), 7.10 (d, J = 8.05 Hz, 1H), 7.04 (d, J = 11.7 Hz, 1H), 2.52 (tt, J = 9.15 Hz, J = 3.15 Hz, 1H), 1.96 – 1.85 (m, 4H), 1.50 – 1.38 (m, 2H), 1.38 – 1.26 (m, 3H), 1.26 – 1.19 (m, 2H), 1.12 – 1. 01 (m, 2H), 0.91 (t, J = 7.30 Hz, 3H). A phase transition temperature of compound (1-1-25) obtained was as described below. Phase transition temperature: C 104 N 125 I.

The synthetic route of 4-Bromo-2-fluorobenzotrifluoride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JNC Corporation; JNC Petrochemical Corporation; EP2522649; (2012); 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. 766-46-1, name is 2′-Bromophenylacetylene, A new synthetic method of this compound is introduced below., name: 2′-Bromophenylacetylene

General procedure: All reactions were carried out under aerobic conditions. A mixture of aromatic alkyne (1.0 mmol), AgNO3 (0.075 mmol), Cs2CO3 (1.0 mmol), catalyst compound 1 (0.5 mol %), and n-butyl alcohol/H2O (in 1:2 proportion, 3 mL) was stirred at 60 C for 24 h and then extracted three times with ethyl acetate (3 x 15 mL). The combined organic phase was dried with MgSO4, filtrated, and then solvent was removed on a rotary evaporator. The product was isolated by thin-layer chromatography. The purified products were identified by 1H-NMR and 13C-NMR spectroscopy (Figures S1-S10).

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:
Article; Guo, Mengping; Chen, Bo; Lv, Meiyun; Zhou, Xiuling; Wen, Yongju; Shen, Xiuli; Molecules; vol. 21; 5; (2016);,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 55289-36-6, A common heterocyclic compound, 55289-36-6, name is 3-Bromo-2-methylaniline, molecular formula is C7H8BrN, 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.

Intermediate 32C: N-(3-Bromo-2-methylphenyl)-2-(3-methoxypyridin-2-yl)acetamide A mixture of sodium 2-(3-methoxypyridin-2-yl)acetate (0.166 g, 0.871 mmol), 3-bromo-2-methylaniline (0.118 mL, 0.958 mmol), DIEA (0.608 mL, 3.48 mmol) and HATU (0.397 g, 1.05 mmol) in DMF (4.0 mL) was stirred at room temperature. After 1 h, the mixture was diluted with EtOAc and washed twice with 10% aqueous LiCl, then with brine, dried and concentrated. The residue was purified by column chromatography on silica gel to provide N-(3-bromo-2-methylphenyl)-2-(3-methoxypyridin-2-yl)acetamide as a pale yellow solid (0.213 g, 73% yield). Mass spectrum m/z 335, 337 (M+H)+.

The synthetic route of 55289-36-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Batt, Douglas G.; Bertrand, Myra Beaudoin; Delucca, George; Galella, Michael A.; Ko, Soo Sung; Langevine, Charles M.; Liu, Qingjie; Shi, Qing; Srivastava, Anurag S.; Tino, Joseph A.; Watterson, Scott Hunter; US2014/378475; (2014); 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. 337915-79-4, name is 5-Bromo-N1-methylbenzene-1,2-diamine, A new synthetic method of this compound is introduced below., SDS of cas: 337915-79-4

Step C6-bromo- 1 -methyl- 1 H-benzimidazol-2-[00304] A solution of (2-amino-5-bromophenyl)methylamine (992 mg, 4.93 mmol) inMeOH (10 mL) was treated with cyanogen bromine (1045 mg, 9.87 mmol). The reaction mixture was maintained at room temperature for 1 h, then partitioned between EtOAc (100 mL), a sat. NaHC03 solution (100 mL) and water (20 mL). The organic layer was washed with a sat. NaCI solution, dried (Na2S04) and concentrated. The residue was triturated using CH2CI2 to obtain 6- bromo-1-methyl-1 H-benzimidazol-2-amine (952 mg, 4.21 mmol, 85 % yield) as a beige solid:.1H NMR (400 MHz, DMSO-cfe) delta ppm 3.48 (s, 3 H) 6.57 (s, 2 H) 7.04 (d, J=0.98 Hz, 2 H) 7.30 – 7.38 (m, 1 H) ES LC-MS m/z =226.1 (Br79, M+H)+; ES LC-MS m/z =228.1 (Br81, M+H)+.

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; GLAXOSMITHKLINE LLC; BOTYANSZKI, Janos; DICKERSON, Scott Howard; LEIVERS, Martin Robert; LI, Xiaofei; MCFADYEN, Robert Blount; REDMAN, Aniko Maria; SHOTWELL, John Bradford; XUE, Jianjun; WO2012/174312; (2012); A2;,
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. 50548-45-3, name is 1-Bromodibenzo[b,d]furan, A new synthetic method of this compound is introduced below., category: bromides-buliding-blocks

500ml round bottom flask reactor, 1-bromodibenzofuran(20.0g, 0.081mmol), bis(pinacolato)diboron (26.7g, 0.105mol), [1,1′-bis(diphenylphosphino)ferrocene]palladium dichloride (1.3g, 0.002mol), potassium acetate (19.9g, 0.202mol), into a 1,4-dioxane 200ml were stirred for 10 hours under reflux after completion of the reaction was filtered a pad of celite. Filtrate was concentrated under a reduced pressure was separated and then the column was recrystallized from dichloromethane and heptane to give a intermediate 4-a> (17.0g, 70%).

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; SFC CO LTD; PARK, SEOK BAE; SONG, JU MAN; LEE, YUR IM; KIM, HEE DAE; PARK, SANG WOO; JEONG, KYUNG SEOK; CHA, SOON WOOK; (96 pag.)KR2015/130206; (2015); A;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 17247-58-4, name is (Bromomethyl)cyclobutane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of (Bromomethyl)cyclobutane

Example 5; Preparation of N-cyclobutylmethyl-6,14~endoethano-7-(2-hydroxy-2-cyclobutyl-2-ethyl)-tetrahydronorthebaine (compound (VI); R1 and R2= cyclobutyl); 596 mg (4 mmol) of bromomethyl cyclobutane, 1 g (7.2 mmol) of potassium carbonate and 1 g (2.5 mmol) of the compound of formula (V) obtained in Example 4 were added slowly to 10 ml of dimethylformamide. The resulting mixture was heated to 135 C and stirred for 3 hours. The excess potassium carbonate was removed by filtration, and the solvent was removed by vacuum distillation. The remaining solid was filtered and vacuum dried to obtain the title compound (0.94 g, 81%).

The synthetic route of 17247-58-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; HANMI PHARM. CO., LTD.; WO2006/25710; (2006); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 583-75-5,Some common heterocyclic compound, 583-75-5, name is 4-Bromo-2-methylaniline, molecular formula is C7H8BrN, 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.

4-bromo-2-methylaniline (5.0 g, 27 mmol) was added to a mixture of water (12.3 ml) and HBF4 (48% by weight in water, 12.3 ml, 67 mmol) in a Nalger reaction vessel cooled in an ice water bath. Then, NaNO2 (1.85 g, 27 mmol) in water (3.8 ml) was added while maintaining the temperature of the reaction around 10 C. After 15 minutes, the was then recooled in an ice water bath and filtered via a Buchner funnel. The solid was washed with cold 5% aqueous HBF4, cold MeOH (20 ml) and diethyl ether (3 x 10 ml). The solid was dried on a Buchner funnel for 1 hour and then added to a flask containing KOAc (5.3 g, 54 mmol, dried in vacuo overnight) and 18-C-6 (0.35 g, 1,3 mmol) suspended in chloroform (250 ml). The reaction was stirred at room temperature for 2 hours and then filtered, and the solid was washed with chloroform. The filtrate was washed with water and brine, dried over sodium sulfate, filtered, concentrated, and diluted with water (250 ml). The suspension was filtered, and the solid was washed with hexanes (50 ml) and diethyl ether (50 ml), collected, and dried in vacuo to give title compound (3.6 g, 68%). MS (ESI pos. ion) m/z: 197 (M+H). Calc’d Exact Mass for C7H5BrN2: 196.

The synthetic route of 583-75-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AMGEN INC.; WO2007/5668; (2007); A2;,
Bromide – Wikipedia,
bromide – Wiktionary