Month: August 2021

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. 955959-84-9, name is 4-(4-Bromophenyl)dibenzo[b,d]furan, A new synthetic method of this compound is introduced below., COA of Formula: C18H11BrO

In a stream of nitrogen, was added 2-chlorocarbazole 3.0g (14.9mmol) in 50mL three-necked flask, 1-bromo-4-(4-dibenzofuranyl)benzene, 4.8g (14.9mmol), potassium carbonate 4.1g (29.8mmol), o-xylene 25mL, palladium acetate, 67mg (0.29mmol) and tri (tert-butyl) phosphine 210mg (1.0mmol), stirred at 140 °C 6 hours. After cooling to room temperature, water was added 10mL, the organic layer was separated. The organic layer was washed with water, washed sequentially with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (mixed solvent of toluene and hexane (volume ratio = 1: 2)) was purified, isolated 2-chloro-9-(4-(4-dibenzofuran-yl)phenyl)carbazole as a white powder 5.4g (12.1mmol) (yield 81percent).

The synthetic route of 955959-84-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Tosoh Corporation; Naoki, Matsumoto; Hirokazu, Shinya; (43 pag.)CN105531262; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 55289-36-6, name is 3-Bromo-2-methylaniline, 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. name: 3-Bromo-2-methylaniline

To a vigorously stirred solution of 3-bromo-2-methylaniline (5.0 g, 26.9 mmol) in a 1 :1 mixture of dichloromethane (67.2 mL) and sodium bicarbonate (80.6 mL, 1 .15 M) was added dropwise a solution of triphosgene (2.79 g, 9.41 mmol, 0.35 equiv) in (15 mL) at 0C. The reaction mixture was stirred until no more gas formation was observed. The organic and water phases were separated. The aqueous phase was extracted with dichloromethane, and the combined organic layer was washed with brine, dried over Na2S04 and concentrated under reduced pressure to give 1-bromo-3- isocyanato-2-methyl-benzene (5.70 g, 98 %) as a brown liquid that was used in the next step without further purification. NMR (400 MHz, CDCIs) delta 7.40 (dd, J = 7.9, 1.5 Hz, 1 H), 7.05 (dd, J = 8.0, 1.5 Hz, 1 H), 7.00 (t, J = 7.9 Hz, 1 H), 2.43 (s, 3H). LC (method A): 0.99 min.

The synthetic route of 3-Bromo-2-methylaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SYNGENTA PARTICIPATIONS AG; QUARANTA, Laura; BOU HAMDAN, Farhan; POULIOT, Martin; RENDINE, Stefano; (94 pag.)WO2018/114541; (2018); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 627871-16-3, name is 5-Bromo-4-fluoro-2-methylaniline, belongs to bromides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 627871-16-3, Computed Properties of C7H7BrFN

Alkylation of Compound (H) with Compound (I) to form Compound (G) To a mixture of Compound (I) (1.0 equiv) and Compound (H) (1.1 equiv) in toluene (5 vols) is charged iPr2Et (2.1 equiv). The mixture is heated to about 90 to about 100 C and aged for about less than 10 hours. Upon completion, the mixture is cooled and diluted with water (about 5 to about 6 vols). The biphasic mixture is separated and the organic solution is washed sequentially with aq. H4C1 (about 27 wt%, about 2 to about 3 vols), aq. NaHC03(about 9 wt%, about 2 to about 3 vols), and aq. NaCl (about 15 wt%, about 1 vols). The organic solution is dried over Na2S04, filtered, and washed with toluene (about 2 to about 3 vols). The solution is concentrated under vacuum at about 45 C and the residue is crystallized by the addition of hexane at about 20 C to about 25 C and at about 10 C to about 15 C. The slurry is filtered, washed with cooled isopropanol (about 1 vol) and dried under vacuum at about 37 C to about 43 C to afford Compound (G). 1H NMR (400 MHz, DMSO-d6): delta 7.05 (d, 1H, J= 12.0 Hz), 6.51 (d, lH, J= 8.0 Hz), 5.27 (t, 1H, J= 4.0 Hz), 4.17 (d, 2H, J= 4.0 Hz), 2.21-2.14 (m, 1H), 2.10 (s, 3H), 0.96-0.86 (m, 4H).13C NMR (100 MHz, DMSO-d6): 208.17, 151.63, 149.32, 143.99, 143.97, 123.81, 123.74, 118.13, 117.90, 112.87, 105.09, 104.88, 53.72, 18.33, 17.43, 17.42, 10.85.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Bromo-4-fluoro-2-methylaniline, and friends who are interested can also refer to it.

Reference:
Patent; GILEAD SCIENCES, INC.; BROWN, Brandon Heath; CHAN, Brenda J. Burke; CHIU, Anna; GRIGGS, Nolan; HEUMANN, Lars V.; LATHROP, Stephen P.; REYNOLDS, Troy Evan; SARMA, Keshab; SILER, David Allen; THOMPSON, Andrew S.; WANG, Tao; (146 pag.)WO2016/106384; (2016); A1;,
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. 69272-50-0, name is 3,6-Dibromobenzene-1,2-diamine belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 69272-50-0

In a flask,Intermediate 2-1 (17g, 64.4mmol),Benzil (13.5g, 64.4mmol) and acetic acid (400ml),Stirring,Heated to 90C,Stirring 3h.Cooling to room temperature,Solid separated.filter,The crude product was recrystallized from ethanol,Light yellow powder 21g,75% yield.

The synthetic route of 69272-50-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shanghai Taoe Chemical Technology Co., Ltd.; Huang, Jinhai; Su, Jianhua; (22 pag.)CN105753849; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 73918-56-6, name is 2-(4-Bromophenyl)ethanamine, belongs to bromides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 73918-56-6, Formula: C8H10BrN

General procedure: Compound 3 (0.37 g, 1 mmol), 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide (EDC, 0.29 g,1.5 mmol), 1-hydroxybenzotrizole (HOBT, 0.20 g, 1.5 mmol) and CHCl3 (20 mL) were stirred at roomtemperature for 1 h, and then different amines (3 mmol) were added. The solution was stirred atroom temperature overnight. Then the solvent was poured into water and extracted with ethylacetate (20 mL × 3). The solution was dried over anhydrous Na2SO4 and concentrated. The residues were purified by flash chromatography with chloroform/petroleum ether (2:1, v/v) elution.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-(4-Bromophenyl)ethanamine, and friends who are interested can also refer to it.

Reference:
Article; Li, Bo; Huang, Ai-Ling; Zhang, Yi-Long; Li, Zeng; Ding, Hai-Wen; Huang, Cheng; Meng, Xiao-Ming; Li, Jun; Molecules; vol. 22; 7; (2017);,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 630-17-1, 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. 630-17-1, name is 1-Bromo-2,2-dimethylpropane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

N- (benzyloxycarbonyl) acetamide potassium salt(231 mg, 1.00 mmol) and 18-crown-6 (264 mg, 1.00 mmol)Was dissolved in dimethylformamide (1 mL).After adding 1-bromo-2-chloroethane (83 mL, 1.00 mmol)And the mixture was stirred at room temperature for 19.5 hours.The reaction was terminated by adding saturated aqueous ammonium chloride solution (about 3 mL)The reaction mixture was extracted with ethyl acetate.After washing the organic layer with water and saturated brine,And dried over anhydrous magnesium sulfate.Flash silica gel chromatography(20% ? 40% ethyl acetate / n-hexane)N- (benzyloxycarbonyl) -N- (2-chloroethyl) acetamide(137 mg, 54%) of a colorless oil.

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, 1-Bromo-2,2-dimethylpropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; School corporation Meijo University; Mori, Yuji; Sakai, Takeo; Fukuda, Ayumi; Kasai, Satomi; (28 pag.)JP2018/95576; (2018); A;,
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. 103273-01-4, name is 2-Bromo-4-(tert-butyl)aniline, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 103273-01-4

2-Bromo-4-tert-butyl-phenylamine (162 g, 0.71 mol) was added dropwise to H2SO4 (410 mL) at room temperature to yield a clear solution. This clear solution was then cooled down to -5 to -10 0C. A solution of KNO3 (82.5 g, 0.82 mol) in H2SO4 (410 mL) was added dropwise while the temperature was maintained between -5 to -10 0C. Upon completion, the reaction mixture was poured into ice / water and extracted with EtOAc. The combined organic layers were washed with 5% Na2CO3 and brine, dried over Na2SO4 and concentrated. The residue was purified by a column chromatography (EtOAc / petroleum ether 1 / 10) to give 2- bromo-4-ter£-butyl-5-nitro-phenylamine as a yellow solid (152 g).

According to the analysis of related databases, 103273-01-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; VERTEX PHARMACEUTICALS INCORPORATED; WO2009/36412; (2009); A1;,
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. name: (Bromomethyl)cyclobutane

Step 1. EPO A stirred solution of the ketimime 1a’ (50 g, 187.1 mmol, available from Aldrich Chemical Company, Milwaukee, Wisconsin) under N2 in dry THF (400 ml_) was cooled to -780C and treated with 1 M solution of K-4BuO (220 ml_, 1.15 equiv.) in THF. The reaction mixture was warmed to 0 C and stirred for 1 h and treated with bromomethylcyclobutane (28 mL, 249 mmol). The reaction mixture was stirred at room temperature for 48 h and concentrated in vacuo. The residue was dissolved in Et2O (300 mL) and treated with aq. HCI (2 M, 300 mL) The resulting solution was stirred at room temperature for 5 h and extracted with Et2O (1 L). The aqueous layer was made basic to pH -12-14 with aq. NaOH (50 %) and extracted with CH2CI2 (3×300 mL). The combined organic layers were dried (MgSO4), filtered, and concentrated to give pure amine (1b’, 18 g) as a colorless oil

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

Reference:
Patent; SCHERING CORPORATION; WO2006/130688; (2006); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

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 1159977-65-7 as follows. COA of Formula: C6H4BrN3

To a mixture of 2,4-difluoro-N-(2-methoxy-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-3-yl)benzenesulfonamide (2.13 g, 5.0 mmol), 6-bromoimidazo[1,2-b]pyridazine (1 g, 0.79 mmol), Pd(dppf)Cl2.CH2Cl2 (408 mg, 0.5 mmol) and Na2CO3 (1.32 g, 12.5 mmol) were added DME (120 mL) and water (30 mL). The mixture was stirred at 70 C. under N2 atmosphere for 4 hours, then cooled to rt, quenched with H2O (500 mL), and then extracted with EtOAc (500 mL*3). The combined organic phases were concentrated in vacuo. The residue was purified by a silica gel column chromatography (DCM/MeOH (v/v)=200/3) to give the title compound as a light brown solid (1.28 g, 61.4%). MS (ESI, pos. ion) m/z: 418.0 [M+H]+.

According to the analysis of related databases, 1159977-65-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Calitor Sciences, LLC; Xi, Ning; US2014/134133; (2014); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 586-61-8,Some common heterocyclic compound, 586-61-8, name is 1-Bromo-4-isopropylbenzene, molecular formula is C9H11Br, 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.

General procedure: A sealable reaction tube was charged with azole (0.75 mmol),aryl bromide (0.50 mmol), [(NHC)Pd(h3-allyl)]2(m2-N-heterocycle)(BF4)2 (0.0025 mmol), LiOtBu (1.0 mmol) and DME (4.0 mL).The mixture was stirred at 100 C for 12 h. After completion of thereaction, the filtrate was concentrated and the residue was subjectedto purification via column chromatography to give the correspondingproduct.

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-isopropylbenzene, its application will become more common.

Reference:
Article; Yang, Jin; Tetrahedron; vol. 75; 14; (2019); p. 2182 – 2187;,
Bromide – Wikipedia,
bromide – Wiktionary