Tag: M.W=100-200

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., SDS of cas: 39478-78-9

A solution of concentrated sulphuric acid (6ml_) in distilled water (75ml_) was added to 5- bromo-2-methylaniline (1g, 5.38mmol). The resultant suspension was heated to 9O0C and stirred for 4.5h. The reaction mixture was then cooled using an ice bath and a solution of sodium nitrite (384mg, 5.57mmol) in water (5ml_) was added to the reaction mixture at O0C. The reaction was then allowed to warm to ambient temperature. The reaction mixture was then added to a solution of concentrated sulphuric acid (6ml_) in water (75ml_) which had been preheated to 9O0C. The reaction mixture was stirred for 1 h at 9O0C and allowed to cool, on standing, overnight. A precipitate was observed in the reaction mixture. The precipitate was collected by filtration, washed with water, and dried in a vacuum oven to afford 5-bromo-2-methylphenol as a brown solid (510mg, 2.73mmol, 51 %). M.S. (ESI) (m/z) 185, 187[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; N.V. ORGANON; WO2007/63071; (2007); 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. 2550-36-9, name is (Bromomethyl)cyclohexane, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H13Br

The compound prepared in Step 5 (35 mg, 0.08 mmol), (bromomethyl) cyclohexane (21 mg, 0.12 mmol), K2C03 (22 mg, 0.16 mmol), KI (2 mg) in DMF (2 mL) was stirred at 90C for 16 hours under N2. The mixture was concentrated, diluted with DCM, washed with brine, dried over Na2SC>4, filtered and the solvent was evaporated. The residue was purified by prep-HPLC to give pure product (15 mg, yield: 35%). 1H-NMR (400 MHz, CDCI3) delta 7.97-7 93 (m, 2H), 7.73 (s, 1H), 7.58 (s, 1H), 7.52-7.50 (m, 2H), 7.44-7.37 (m, 3H), 7.24-7.16 (m, 2H), 5.84 (s, 1H), 3.18-3.13 (m, 1H), 2.99-2.97 (m, 4H), 2.95 (s, 3H), 1.74-1.58 (m, 1H),1.54~1.51 (m, 2H), 1.43-1.41 (m, 2H), 1.04-0.91 (m, 4H), 0.89-0.79 (m, 2H), 0.76-0.56 (m, 1H). MS (M+H)+: 535.

The synthetic route of 2550-36-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; ISTITUTO DI RICERCHE DI BIOLOGIA MOLECOLARE P. ANGELETTI, SRL; MCCOMAS, Casey Cameron; LIVERTON, Nigel, J.; HABERMANN, Joerg; KOCH, Uwe; NARJES, Frank; LI, Peng; PENG, Xuanjia; SOLL, Richard; WU, Hao; WO2011/106929; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 53078-85-6, 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 53078-85-6 as follows.

General procedure: A dried tube, equipped with a magnetic stirred and a septum, 2-bromoaniline (0.17 g,1.0mmol) was dissolved in DMSO (3mL), KOt-Bu (0.34 g, 3mmol) was added. The mixturewas stirred for 5 min, and then dithiocarbamate (0.296 g, 1.5mmol) and copper oxide(6.4mg, 8 mmol%) were added. The reaction mixture was heated at 100C and checkedby TLC until the starting material was finished. The reaction mixture was cooled downto room temperature, and then quenched with sat. NH4Cl solution (5mL) and extractedwith ethyl acetate, dried over anhydrous Na2SO4 and concentrated under vacuum. The residue was purified by flash column chromatography to afford the desired product(144mg, 81%).

According to the analysis of related databases, 53078-85-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Xu, Wan; Zeng, Meng-Tian; Liu, Min; Liu, Xing; Chang, Cai-Zhu; Zhu, Hui; Dong, Zhi-Bing; Journal of Sulfur Chemistry; vol. 38; 6; (2017); p. 644 – 654;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 1073-39-8, A common heterocyclic compound, 1073-39-8, name is 3-Bromobicyclo[4.2.0]octa-1,3,5-triene, molecular formula is C8H7Br, 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.

A magnetic stir bar and 3.10 g of magnesium strip were added to the reactor.The vacuum was purged with nitrogen three times (to ensure the removal of oxygen in the system), and 6 mL of tetrahydrofuran and 0.010 g of iodine activated magnesium strip were added to the reactor under nitrogen protection.20 g of 4-bromobenzocyclobutene was diluted in 36 mL of tetrahydrofuran to obtain a mixed solution.A few drops of the mixed solution was added dropwise at room temperature, and the reaction was initiated by contact with magnesium strips and iodine. After the reaction of tetrahydrofuran was slightly refluxed, the mixed solution was slowly added dropwise, and the addition was completed in 2 hours.After the addition was completed, the system was transferred to a 70 C oil bath for 2 h. The temperature was lowered to room temperature under a nitrogen atmosphere, and 14 g of dimethylvinylchlorosilane was diluted in 30 mL of tetrahydrofuran to obtain a mixed solution.The mixture was slowly added dropwise to the human system, and the addition was completed in 2 hours. After the completion of the dropwise addition, the system was transferred to a 70 C oil bath, and the reaction was continued for 2.5 h to obtain an off-white slurry.Separation and purification: After the reaction is completed, the obtained off-white slurry is cooled to room temperature.The excess Grignard reagent was quenched by the addition of 3 mol/L of dilute hydrochloric acid (the amount of dilute hydrochloric acid added was allowed to react the remaining magnesium strips in the reaction).It was extracted with 25 mL of n-hexane, extracted three times, and the organic phases were combined. After washing with dilute hydrochloric acid, saturated aqueous sodium hydrogencarbonate solution and saturated aqueous sodium chloride solution,It was dried over anhydrous sodium sulfate for 5 h. Filtration and concentration of the filtrate on a rotary evaporator afforded a pale yellow liquid.The liquid was subjected to distillation under reduced pressure and a fraction having a temperature of 80 C was collected to obtain a colorless transparent liquid, which was a 4-dimethylvinylsilylbenzocyclobutene (4-DMVSBCB).

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; Southwest University of Science and Technology; Yang Junxiao; Wei Xuelian; Yin Qiang; Hu Huan; Li Xian; Fan Li; Ma Jiajun; (14 pag.)CN108503664; (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. 2924-09-6, name is 5-Bromo-2-fluoroaniline, This compound has unique chemical properties. The synthetic route is as follows., category: bromides-buliding-blocks

A mixture of 5-bromo-2-fluoroaniline (10 g, 52.6 mmol), 3- (trifluoromethyl)benzene-1-sulfonyl chloride (12.9 g, 52.6 mmol) and pyridine (30 mL) was stirred overnight at 60oC. The pH value of the solution was adjusted to 3-4 with 1M aqueous hydrogen chloride. The mixture was extracted three times with dichloromethane. The combined organic layers combined were dried (Na2SO4) and concentrated. The residue was purified via MPLC eluting with 10% ethyl acetate in petroleum ether to afford N-(5-bromo-2- fluorophenyl)-3-(trifluoromethyl)benzenesulfonamide (19.3 g, 92%) as a light yellow solid.

According to the analysis of related databases, 2924-09-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; LYCERA CORPORATION; AICHER, Thomas, Daniel; TAYLOR, Clarke, B.; VANHUIS, Chad, A.; (410 pag.)WO2016/201225; (2016); 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. 1003-98-1, name is 2-Bromo-4-fluoroaniline, This compound has unique chemical properties. The synthetic route is as follows., category: bromides-buliding-blocks

Step 1: 2-(2-Bromo-4-fluorophenyl)hydrazinium chlorideTo a suspension of 2-bromo-4-fluoroaniline in concentrated HCl (1.5M) at -10 0C was slowly added a 10.0M aqueous solution OfNaNO2 (1.1 eq). The mixture was stirred at O 0C for 2.5 hrs. A cold (-30 C) solution Of SnCl2 (3.8M) in concentrated HCl was then slowly added while maintaining the internal temperature below 10 0C. The resulting mixture was stirred mechanically for 20 mm at 10 C, then at room temperature for 1 hr. The thick slurry was filtered and the solid was air dried overnight. The solid was resuspended in cold HCl and filtered again. The dried material was suspended in Et2O, stirred for 10 min, filtered and air dried overnight to give the title compound as a beige solid

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 1003-98-1.

Reference:
Patent; MERCK & CO., INC.; WO2006/89309; (2006); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

7073-94-1, name is 1-Bromo-2-isopropylbenzene, 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. Formula: C9H11Br

29.87 g 1-bromo-2-isopropyl benzene and 23.6 g 2-naphthylamine were added into a dry 2 L three-neck flask, followed by adding 600 mL dry and degassed toluene to dissolve. Then, 43.2 g sodium tert-butoxide (3.0 eq.), 0.7 g catalyst palladium diacetate (2% mol) and 3.7 g 1,1?-binaphthyl-2,2?-bis(diphenylphosphino) (BINAP, 4% mol) ligand were added. The reaction mixture was heated up to 110 C. and reacted overnight. After the reaction finished and the reaction mixture was cooled down to room temperature. The residual was absorbed by the added activated carbon, filtered by suction filtration and removed with solvent by rotary evaporation, followed by recrystallization with a mixture of toluene and ethanol, to produce 34.5 g Intermediate (18) at a yield of 88%.

The synthetic route of 7073-94-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NANJING TOPTO MATERIALS CO.,LTD.; KIM, JIN WOO; QIAN, CHAO; GAO, PENGHUI; WANG, XIAOWEI; (157 pag.)US2018/105534; (2018); A1;,
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 2695-48-9 as follows. COA of Formula: C8H15Br

[0130] 133 mmol of 1 1 -bromo1 -undecene and 136 mmol of triethoxy silane were added to a single neck RBF attached with an attached reflux condenser. Then 1 .0 mL Karstedt’s catalyst (2 Wt. % solution in toluene, 0.1 mmol)) was added via syringe and flask was in the oil bath between 70C for 2h. Separation of (8-bromooctyl) triethoxysilane from rearrangement olefin and excess triethoxy silane was achieved by fractional distillation under high vacuum (BP. 170C at 10″6mm). Yield 53.3%. FIG. 1 shows the 1H NMR spectrum of (8-bromooctyl) triethoxysilane.

According to the analysis of related databases, 2695-48-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK PATENT GMBH; BOBADE, Sachin; POLISHCHUK, Orest; PADMANABAN, Munirathna; BASKARAN, Durairaj; (65 pag.)WO2019/81450; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 452-74-4, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 452-74-4 name is 1-Bromo-2-fluoro-4-methylbenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

1-Bromo-2-fluoro-4-methyl-5-nitrobenzene HNO3 (9 mL) was added into a solution of 1-bromo-2-fluoro-4- methylbenzene (5.35 g, 28.30 mmol) in H2SO4 (25 mL) while it was kept at -20 C and the resulting mixture was stirred at 0 C for 10 min. The mixture was poured into ice- water and extracted with ethyl acetate. The organic layer was washed with saturated NaHCO3 aqueous solution and brine, dried over Na2SO4 and concentrated in vacuo to yield the product as a yellow solid (5.3g, 80 % yield).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-2-fluoro-4-methylbenzene, and friends who are interested can also refer to it.

Reference:
Patent; ARAXES PHARMA LLC; LI, Liansheng; FENG, Jun; WU, Tao; REN, Pingda; LIU, Yi; LIU, Yuan; LONG, Yun, Oliver; WO2015/54572; (2015); 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. 2550-36-9, name is (Bromomethyl)cyclohexane, A new synthetic method of this compound is introduced below., Recommanded Product: (Bromomethyl)cyclohexane

Example 4A 3-(Cyclohexylmethoxy)pyridine-2-amine At RT, 96 g of sodium hydroxide, 45% strength in water (1081 mmol, 1 equivalent), were initially charged in 1170 ml of methanol, 119 g of 2-amino-3-hydroxypyridine (1080 mmol, 1 equivalent) were added and the mixture was stirred at RT for another 10 min. The reaction mixture was concentrated under reduced pressure, the residue was taken up in 2900 ml of DMSO and 101 g of cyclohexylmethyl bromide (1135 mmol, 1.05 equivalents) were added. After 16 h at RT, the reaction mixture was slowly added to 6 l of water and the aqueous solution was extracted twice with in each case 21 of ethyl acetate. The combined organic phases were washed with in each case 1 l of saturated aqueous sodium bicarbonate solution and water, dried, filtered and concentrated. The residue was stirred with 500 ml of n-pentane, filtered and dried under reduced pressure. This gave 130 g (58% of theory) of the title compound. LC-MS (Method 3): Rt=1.41 min MS (ESpos): m/z=207.1 (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; Bayer Pharma Aktiengesellschaft; VAKALOPOULOS, Alexandros; BUCHGRABER, Philipp; LINDNER, Niels; FOLLMANN, Markus; WUNDER, Frank; STASCH, Johannes-Peter; MARQUARDT, Tobias; REDLICH, Gorden; DIETZ, Lisa; LI, Volkhart Min-Jian; (81 pag.)US2017/217954; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary