Tag: M.W=100-200

Related Products of 17247-58-4,Some common heterocyclic compound, 17247-58-4, name is (Bromomethyl)cyclobutane, 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.

A stirred solution of the ketimime 1a’ (50 g, 187.1 mmol, available from Aldrich Chemical Company, Milwaukee, Wis.) under N2 in dry THF (400 mL) was cooled to -78 C. and treated with 1 M solution of K-tBuO (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. HCl (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 CH2Cl2 (3×300 mL). The combined organic layers were dried (MgSO4), filtered, and concentrated to give pure amine (1b’, 18 g) as a colorless oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route (Bromomethyl)cyclobutane, its application will become more common.

Reference:
Patent; Schering Corporation; US2006/276405; (2006); 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. 39478-78-9, name is 5-Bromo-2-methylaniline, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H8BrN

Example 1.Preparation of 2-methyl-5-bromophenylguanidine nitrate of the Formula 3; Preparation of 5-bromo-2-methylaniline hydrochlorideA 5-L reactor has been charged with 812.3 g of 5-bromo-2-methylaniline (4.36 mol. 1.0 eq), and 3.7 kg of methylene chloride. After cooling the obtained clear solution to 1O0C, 190.7 g of dry hydrogen chloride gas was added from a bottle over a period of 2.5 h. The resulting mixture was stirred for ca. 30 minutes, whereafter the obtained crystalline product was filtered off on a filter funnel. The precipitate was washed on a filter funnel with two portions of methylene chloride (200 g each). The product was dried at room temperature for 3 days to yield 976.4 g of 5-bromo-2-methylaniline hydrochloride (100%) having an HPLC purity of 99.6%.

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; TEMAPHARM SP. z o.o.; GRUZA, Henryk; MIREK, Slawomir; JEZEWSKI, Artur; WRZOSEK, Artur; WO2010/14022; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 656-64-4, name is 3-Bromo-4-fluoroaniline, 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 656-64-4, HPLC of Formula: C6H5BrFN

Compound 3 (5 g, 30.9 mmol) was dissolved in 50 mL water and heated to 65 C.Further, Compound 4 (6.5 g, 34.0 mmol) was added, and then a saturated sodium hydrogen carbonate solution (50 mL) was added dropwise.After reacting for 1 hour, it was extracted with ethyl acetate, dried over anhydrous sodiumThe petroleum ether was passed through a column of ethyl acetate (4:1) to afford compound 5 (9 g, 92%) as white solid.

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, 3-Bromo-4-fluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Shanghai Xiangjin Biological Technology Co., Ltd.; Sun Fang; Zhan Youni; (38 pag.)CN109574950; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 452-74-4, 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. 452-74-4, name is 1-Bromo-2-fluoro-4-methylbenzene, This compound has unique chemical properties. The synthetic route is as follows.

A degassed solution of 3-amino-furo[3,2-c]pyridine-2-carboxylic acid ethyl ester (300 mg, 1.46 mmol), 4-bromo-3-fluorotoluene (277 mul, 2.19 mmol), Pd2dba3 (67 mg, 0.073 mmol), Xantphos (84 mg, 0.15 mmol) and potassium phosphate tribasic (620 mg, 2.92 mmol) in toluene (10 ml) was heated at reflux under an argon atmosphere for 16 hours. The reaction mixture was concentrated in vacuo and the residue was purified by flash chromatography (Si-SPE, pentane: diethyl ether, gradient 100:0 to 75:25) to afford the title compound as a yellow solid (252 mg, 55%). LCMS (method B): Rx = 3.14 min, M+H+ = 315.

The chemical industry reduces the impact on the environment during synthesis 1-Bromo-2-fluoro-4-methylbenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; GENENTECH, INC.; WO2008/24725; (2008); 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. 583-70-0, name is 2,4-Dimethylbromobenzene, A new synthetic method of this compound is introduced below., COA of Formula: C8H9Br

General procedure: A flask furnishedwith a dropping funnel was charged with the aryl/alkylbromide in Et2O. n-BuLi(1.6 M in hexane) diluted with Et2O was added dropwise at -78C. After addition, thereaction was kept at -78C for 10 min and was then allowed to warm to room temperatureand stirred for 30 min. The solution was transferred via cannula to SiCl4 dissolved in Et2Oat 0C. The reaction was stirred for 2 h and was allowed to warm to room temperature. Thesolvent was removed under reduced pressure and the residue dissolved in boiling toluene.Insoluble salts were removed via filtration through cellite and washed with hot toluene. Thesolvent from the resulting clear solution was removed under reduced pressure, followed bypurification via distillation or recrystallization.

The synthetic route of 583-70-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Binder, Judith; Fischer, Roland C.; Flock, Michaela; Torvisco, Ana; Uhlig, Frank; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 190; 11; (2015); p. 1980 – 1994;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 54879-20-8, 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. 54879-20-8, name is 2-Bromo-3-methylaniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 2-bromo-3-methylaniline (1.0 eq.) in tetrahydrofuran (0.2 M) at 0° C. under N2 atmosphere was added dropwise 1M NaHMDS (2.5 eq.). The reaction was stirred for 15 minutes at 0° C., and a solution of di-tert-butyl dicarbonate in tetrahydrofuran was added. The reaction was warmed to room temperature overnight. The solvent was evaporated, and the resulting residue was quenched with 0.1N HCl aqueous solution. The aqueous suspension was extracted twice with ethyl acetate. The combined organic layers were washed with brine, dried over anhydrous MgSO4, and concentrated en vacuo. The crude material was purified by flash chromatography on a COMBIFLASH® system (ISCO) using 0-5percent ethyl acetate in hexane to give product as light yellow oil.

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

Reference:
Patent; GlaxoSmithKline Biologicals SA; Skibinski, David; Jain, Siddhartha; Singh, Manmohan; O’Hagan, Derek; (124 pag.)US9408907; (2016); B2;,
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. 4333-56-6, name is Bromocyclopropane, A new synthetic method of this compound is introduced below., HPLC of Formula: C3H5Br

[000459j A mixture of Compound 19A (2.0 g, 10 mmol), bromocyclopropane (2.4 g, 20 mmol), Cs2CO3 (9.8 g, 30 mmol) in DMSO (40 mL) was stirred at 170 C for 2 days under high pressure. The mixture was cooled to room temperature and filtered through celite. The filtrate was diluted with ethyl acetate (100 mL), washed with brine (100 mL x 2), dried over sodium sulfate, and concentrated. The crude was purified with column chromatography on silica gel (petroleum ether, 100% v/v) to render Compound 19B. LC-MS (mlz): 247 [M+1] ?H-NMR (CDC13, 400 MHz) major characteristic peaks: 5 (ppm) 0.78-0.82 (m, 4H), 3.7 1-3.73 (m, 1H), 6.95-6.95 (m, 1H), 7.13-7.18 (m, 1H), 7.34-7.36 (m, 1H).

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

Reference:
Patent; BIOMARIN PHARMACEUTICAL INC.; WANG, Bing; WO2015/65937; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 17247-58-4, The chemical industry reduces the impact on the environment during synthesis 17247-58-4, name is (Bromomethyl)cyclobutane, I believe this compound will play a more active role in future production and life.

Example 1268: 2-(5-Chloro-6-(2,2,2-trifluoroethoxy)-4′-(trifluoromethyl)biphenyl-3-yl)- 3-cyclobutylpropanoic acid Step lEthyl 2-(5-chloro-6-(2,2,2-trifluoroethoxy)-4′-(trifluoromethyl)biphenyl-3-yl)- 3- cyclobutylpropanoate Ethyl 2-(5-chloro-6-(2,2,2-trifluoroethoxy)-4′-(trifluoromethyl)biphenyl-3-yl)acetate (0.6g, 0.49 mmol) was dissolved in anhydrous DMF (3OmL), NaH (60% wt. in paraffin oil, 0.039 g, 1.69 mmol) was added at 00C. The reaction mixture was stirred for 30 min at room temperature and cyclobutylmethyl bromide (0.223 g, 1.49 mmol) was added drop wise at 0 0C. The reaction mixture was stirred an additional Ih at 0 0C and saturated NH4CI solution (1OmL) was added. The reaction mixture was extracted with EtOAc (3x20mL) and the combined organic phases were washed with water (3x20mL) and brine (2OmL), and dried over MgStheta4 The volatiles were removed under reduced pressure and the residue was purified by flash column chromatography to yield ethyl 2-(5-chloro-6- (2,2,2-trifluoroethoxy)-4′-(trifluoromethyl)biphenyl-3-yl)- 3-cyclobutylpropanoate (0.25 g) as a colorless liquid.

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, (Bromomethyl)cyclobutane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ENVIVO PHARMACEUTICALS, INC.; WO2009/86277; (2009); 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. 656-64-4, name is 3-Bromo-4-fluoroaniline, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 3-Bromo-4-fluoroaniline

N-Hydroxy-4-[(2-methoxyethyl)amino]-1,2,5-oxadiazole-3-carboximidoyl chloride (46.0 g, 0.208 mol) was mixed with water (300 mL). The mixture was heated to 60 C. 3-Bromo-4-fluoroaniline [Oakwood products, product No.013091] (43.6 g, 0.229 mol) was added and stirred for 10 min. A warm sodium bicarbonate (26.3 g, 0.313 mol) solution (300 mL water) was added over 15 min. The reaction was stirred at 60 C. for 20 min. LCMS indicated reaction completion. The reaction solution was cooled to room temperature and extracted with ethyl acetate (2*300 mL). The combined ethyl acetate solution was dried over sodium sulfate and concentrated to give the desired product (76.7 g, 98%) as a crude brown solid. LCMS for C12H14BrFN5O3 (M+H)+: m/z=374.0, 376.0. 1H NMR (400 MHz, DMSO-d6): delta 11.55 (s, 1H), 8.85 (s, 1H), 7.16 (t, J=8.8 Hz, 1H), 7.08 (dd, J=6.1, 2.7 Hz, 1H), 6.75 (m, 1H), 6.14 (t, J=5.8 Hz, 1H), 3.48 (t, J=5.2 Hz, 2H), 3.35 (dd, J=10.8, 5.6 Hz, 2H), 3.22 (s, 3H).

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 656-64-4.

Reference:
Patent; Incyte Corporation; Incyte Holdings Corporation; Combs, Andrew P.; Yue, Eddy W.; Sparks, Richard B.; Zhu, Wenyu; (63 pag.)US9320732; (2016); B2;,
Bromide – Wikipedia,
bromide – Wiktionary

656-64-4, name is 3-Bromo-4-fluoroaniline, 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. category: bromides-buliding-blocks

The compound 4-amino-N-hydroxy-1,2,5-oxadiazol-3-carboxamidine Int-1a (20 g, 123.4 mmol, prepared by the method disclosed in the patent application “WO2010005958”) is dissolved in acetic acid Ethyl ester (100mL)And water (100mL),Add 3-bromo-4-fluoroaniline (23.2 g, 123.4 mmol),Sodium bicarbonate (15.5 g, 185.1 mmol),Heat to 60 C, react for 3 hours,The mixture was cooled and EtOAc (EtOAc m.The title compound Int-1b (38 g, 120.9 mmol) was obtained in a yield of 98%.

The synthetic route of 656-64-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shanghai Huahuituo Pharmaceutical Technology Co., Ltd.; Zhejiang Huahai Pharmaceutical Co., Ltd.; Xu Xin; Zhang Tian; Li Yunfei; Wang Guan; Zhu Weibo; Li Dongsheng; Qin Chenggang; Liu Chuanduo; Liu Lei; Wu Qimei; Yang Xuqin; Jia Jie; Wang Ying; Chen Yuhao; Wang Yijin; Ge Jian; (143 pag.)CN109897011; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary