Tag: M.W=200-300

Related Products of 69321-60-4, 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 69321-60-4 as follows.

3-Bromo-2-methylbenzonitrile This compound was prepared in a manner similar to that described for 3-bromo-5-fluorobenzonitrile from commercially available 2,6-dibromotoluene (1.80 g, 7.20 mmol), DMF (11 mL), pyridine (1.1 mL), and copper (I) cyanide (0.52 g, 5.76 mmol). The crude product was purified by flash column chromatography (100 mL silica, hexane) to afford 50 mg (35%) of 3-bromo-2-methylbenzonitrile.

According to the analysis of related databases, 69321-60-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Ligand Pharmaceuticals Incorporated; US5693646; (1997); A;; ; Patent; Ligand Pharmaceuticals Incorporated; US5693647; (1997); A;; ; Patent; Ligand Pharmaceuticals Incorporated; US5696127; (1997); 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, HPLC of Formula: C8H10BrN

To a solution of 2-(4-bromophenyl)ethan-1-amine (5.0 g, 25.0 mmol) in dichloroethane (100 ml), triethylamine (7.0 mL) and trifluoroacetic acid anhydride (7.88 g, 37.5 mmol) were added under ice cooling, and the mixture was stirred for 1 hour. Thereafter, the mixture was stirred at room temperature for further 3 hours. Under ice cooling, water was added to the reaction solution and, after stirring for 20 minutes, the mixture was extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium bicarbonate, a saturated aqueous solution of ammonium chloride, and a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was dissolved in acetic acid (15 mL), fuming nitric acid (30 mL) was slowly added dropwise under ice cooling, and, thereafter, the reaction mixture was stirred under ice cooling for 1 hour and at room temperature for 16 hours. The reaction solution was poured onto ice and extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium bicarbonate and a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by flash column chromatography to obtain N-[2-(4-bromo-3-nitrophenyl)ethyl]-2,2,2-trifluoroacetamide (5.17 g)

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:
Patent; TEIJIN PHARMA LIMITED; US2012/46467; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 103273-01-4, 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 103273-01-4 as follows.

45.0 g (197.26 mol) of Intermediate 21, 33.7 g (197.26 mol) of 2-methoxybenzoyl chloride and 650 mL of THF were added and the mixture was stirred at room temperature for 3 hours. After the reaction was completed, the solvent was distilled off under reduced pressure. And solidified with diisopropyl ether (IPE) to obtain 63.8 g (yield: 89.3%) of a white solid compound (intermediate (22)).

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; Samsung Display Co., Ltd.; Raepto Co., Ltd.; Cho Hwan-hui; Bae Seong-su; Oh Yu-jin; Kim Gyu-ri; Jeong Hye-in; Han Gap-jong; Kim Nam-ho; Kim Hye-jeong; (64 pag.)KR2019/25788; (2019); A;,
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 2255-80-3 as follows. name: 4-Bromo-7-methylbenzo[c][1,2,5]thiadiazole

A mixture of compound (1) 4-Bromo-7-methyl-benzo[1,2,5]thiadiazole (4.582 g, 20.00 mmol), tributyl-thiophen-2-yl-stannane (8.956 g, 24.00 mmol) and 3.0 mol % of tetrakis(triphenylphosphine) palladium [Pd(PPh3)4] (0.693 g, 0.600mmol) in N,N-dimethylformamide (DMF) was stirred for 24 hours at 90 C under N2 atmosphere. A portion of 100mLof water was added the mixture and allowed to cool to room temperature. The mixture was extracted with ethyl acetate (EA) and the extracted organic layer was dried over anhydrous MgSO4. The organic solvent was removed by using a rotary evaporator. The crude product was purified by column chromatography on silica gel using EA/n-hexane. The yield of dark brown liquid was 4.820 g (77.95%). 1H-NMR (400 MHz, CDCl3, ppm): delta 8.05?8.04 (dd, J1 = 3.2 Hz, J2 =2.1 Hz, 1H), 7.76?7.74 (d, J = 6.9 Hz, 1H), 7.42?7.37 (m,1H), 7.19?7.16 (dd, J1 = 5.1 Hz,J2 = 3.6 Hz, 1H), 2.75 (s, 3H). 13C NMR (100 MHz, CDCl3, ppm): delta 156.75, 152.82, 139.59,130.35, 128.31, 127.84, 126.93, 126.64, 125.86, 125.08, 17.92. Anal. Calcd. for C11H8N2S2: C,56.87; H, 3.47; N, 12.06; S, 27.60. Found: C, 56.77; H, 3.39; N, 12.02; S, 27.53.

According to the analysis of related databases, 2255-80-3, the application of this compound in the production field has become more and more popular.

Reference:
Article; Sylvianti, Nadhila; Marsya, Mutia Anissa; Kim, Youn Hwan; Park, Chan-Young; Chang, Dong Wook; Moon, Doo Kyung; Kim, Joo Hyun; Molecular Crystals and Liquid Crystals; vol. 653; 1; (2017); p. 78 – 83;,
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. 327-52-6, name is 1-Bromo-2,4,5-trifluorobenzene, A new synthetic method of this compound is introduced below., Formula: C6H2BrF3

[0113] Into a 100 mL three- necked flask were added 4.62 g 1- bromo- 2, 4, 5- trifluorobenzene (0.022 mol) andanhydrous tetrahydrofuran (50 mL) . The resulting mixture was cooled to- 20 C. The solution of isopropylmagnesiumbromide (22 mmol) in tetrahydrofuran (22 ml, 1 M THF) was slowly added dropwise under nitrogen. After the additionwas completed, the reactants were maintained at- 20 C for later use.[0114] Cuprous bromide – dimethyl sulfide (0.41 g, 0.002 mol) was suspended in 5 ml anhydrous tetrahydrofuran. Theresulting mixture was cooled to -5 C. The Grignard reagent as obtained above was slowly added dropwise undernitrogen. After 15 min, a solution of the acridine compound as shown in the above reaction formula (3.26 g, 0.015 mol)in 30 mL tetrahydrofuran was slowly added dropwise. After additional 5 min, 50 mL saturated solution of ammoniachloride was added to quench the reaction. Into this obtained solution was added 50 mL ethyl acetate for an extraction.The separated water layer was extracted with another 50 mL ethyl acetate. The obtained organic layers were collectedtogether and further washed with saturated solution of sodium chloride and then dried over anhydrous sodium sulfate,followed by filtration and concentration to obtain a crude product which was further treated by column chromatographyto obtain a compound (4.29 g, yield 82%).1H NMR (400 MHz, CDCl3) delta 7.15?6.94 (m, 1 H), 6.88 (d, J = 6.8 Hz, 1H), 4.47 (d, J = 8.9 Hz, 1H), 4.00?3.80 (m, 1 H),2.92?2.76 (m, 1H), 2.76?2.64 (m, 1H), 2.64?2.44 (m, 2H), 2.06 (d, J =14.6 Hz, 3H), 1.84 (s, 1H), 1.66 (qd, J = 14.0, 8.0Hz, 1H), 1.47?1.31 (m, 9H). Ms (M++1): 350.

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; Zhejiang Hisoar Pharmaceutical Co., Ltd; PAN, Xianhua; LI, Weijin; ZHANG, Qunhui; RUAN, Libo; YU, Wansheng; DENG, Fei; MA, Tianhua; HUANG, Mingwang; HE, Minhuan; EP2647624; (2013); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 608-30-0, 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. 608-30-0 name is 2,6-Dibromoaniline, 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.

Under a nitrogen atmosphere, 1.2 mmol alpha,alpha-dione-2,3:5,6-bis(pentamethylene)pyridine, 1.0 mmol of CoCl2, 2.5 mmol of 2,6-dibromoaniline dissolved in 10mL glacial acetic acid, reflux reaction at 120 C (under reflux reaction) for 4 hours. After completion of the reaction, the mixture was cooled to room temperature, and 30 mL of anhydrous ether was added thereto, followed by stirring for 2 hours. Filtered, washed with ether and dried. A brown powder was obtained in a yield of 60.7%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,6-Dibromoaniline, and friends who are interested can also refer to it.

Reference:
Patent; Institute of Chemistry, Chinese Academy of Sciences; Du, Shizhen; Zhang, Wenjuan; Sun, Wenhua; (29 pag.)CN106432356; (2017); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 2255-80-3, name is 4-Bromo-7-methylbenzo[c][1,2,5]thiadiazole, 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 2255-80-3, name: 4-Bromo-7-methylbenzo[c][1,2,5]thiadiazole

Synthesis of Compound A-4-Bromo-7-dibromomethyl-2,1,3-benzothiadiazole A mixture of 4-bromo-7-methyl-2,1,3-benzothiadiazole (45.82 g, 200 mmol), AlBN (6.57 g, 40 mmol), and NBS (106.2 g, 600 mmol) in chlorobenzene (400 mL) was stirred and heated at 80 C. for 4 hours. After cooling to room temperature, the reaction mixture was filtered to remove the solid succinimide, and then the filtrate was washed with water and brine, dried over anhydrous MgSO4, and filtered. The solvent of the filtrate was removed by rotary evaporation, and the crude product was purified by column chromatography on silica gel with CH2Cl2/hexane (v/v, 1:3) as eluent to afford Compound A as a white solid (56.1 g, 83%). The analytical data obtained from Compound A are listed below. M.p. 119-120 C.; IR (KBr) v 3001, 2922, 1524, 1481, 1315, 1274, 1185, 1097, 937, 880 cm-1; 1H NMR (CDCl3, 400 MHz) delta 7.97-7.90 (m, 2H), 7.40 (s, 1H); 13C NMR (CDCl3, 100 MHz) delta 152.8, 149.6, 133.4, 131.8, 129.4, 115.8, 33.9; HRMS (m/z, FAB+) Calcd. for C7H379Br3N2S 383.7567. found 383.7542, Calcd. for C7H379Br281Br1N2S 385.7547. found 385.7553, Calcd. for C7H379Br181Br2N2S 387.7526. found 387.7524, Calcd. for C7H381Br3N2S 389.7506. found 389.7536.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-7-methylbenzo[c][1,2,5]thiadiazole, and friends who are interested can also refer to it.

Reference:
Patent; Wong, Ken-Tsung; Lin, Hao-Wu; Lin, Li-Yen; Lin, Francis; Chen, Yi-Hong; Chiu, Shi-Wen; US8802975; (2014); B2;,
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 24358-62-1 as follows. Safety of 1-(4-Bromophenyl)ethylamine

To a mixture of the compound represented by the structural formula (Q-1) (5.0 g, 25 mmol) and NaOH (2.0 g, 50 mmol) in water (18 mL) and isopropanol (18 mL), the compound represented by the structural formula (Q-1A) (3.31 g, 27.5 mmol) was added dropwise at 20C, and the resulting mixture was stirred at the same temperature for 0.5 hour. Then, the mixture was cooled to 10C, water (50 mL) was added to the mixture, and the resulting mixture was filtered to give white solid. The resulting solid was dissolved in EA (150 mL), and the solution was washed with brine (50 mL), dried over anhydrous sodium sulfate, filtered, and concentrated to give N-[(4-bromophenyl)ethyl]-2,2-dimethylpropanamide as white solid (6.27 g, yield 88%). 1H-NMR Spectrum (300MHz, CDCl3):delta (ppm): 7.43-7.47 (m, 2H), 7.14-7.19 (m, 2H), 5.75 (brs, 1H), 5.02-5.07 (m, 1H), 1.40-1.46 (m, 3H), 1.21 (s, 9H)

According to the analysis of related databases, 24358-62-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Juntendo Educational Foundation; HIRAMATSU Keiichi; MORIMOTO Yuh; BABA Tadashi; HAYAKAWA Isao; (76 pag.)EP2987787; (2016); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 2576-47-8, 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. 2576-47-8, name is 2-Bromoethylamine hydrobromide belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A mixture of aniline (or PhNHEt) (0.05 mol)), 2-bromoethyl- (or 3-bromopropyl)amine hydrobromide and water (6 mL) was heated to 95 C (ina bath), Then, NaHCO3 was added in small portions with stirring. After ~15 min (at 95 C), the reaction mixture was refluxed with stirring using a heating mantle until reaction reached completion. The amount of hydrobromide and NaHCO3 and the timeof heating are given in Table 1. Still warm reaction mixture was diluted with 50% aqueous KOH (11 mL) and water (16 mL). The organic layer was separated, the aqueous layer was saturated with NaCl and extracted with chloroform (4×20 mL), each timeadding NaCl into the aqueous phase. The combined organic layers were dried with MgSO4 and fractionally distilled in vacuo.

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-Bromoethylamine hydrobromide, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Vasilyeva; Vorobyeva; Osipov; Russian Chemical Bulletin; vol. 65; 9; (2016); p. 2211 – 2215; Izv. Akad. Nauk, Ser. Khim.; 9; (2016); p. 2211 – 2215,5;,
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. 937046-98-5, name is 7-Bromopyrrolo[2,1-f][1,2,4]triazin-4-amine, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 7-Bromopyrrolo[2,1-f][1,2,4]triazin-4-amine

To a stirred suspension of Intermediate B (2.50 g, 9.39 mmol) in THF (50 ml_) was added chlorotrimethylsilane (2.98 mL, 23.47 mmol), dropwise. The mixture was stirred at rt for 3 h and 2-propylmagnesium chloride (2M in THF; 24.64 mL, 49.29 mmol) was added dropwise. The suspension immediately went into solution. The mixture was stirred at rt for 3 h and 1-Boc-3-piperidone (3.51 g, 17.60 mmol) was added in one portion. The reaction was stirred at rt for 16 h. The reaction was poured over a mixture of ice and saturated, aqueous ammonium chloride (250 mL). The mixture was allowed to warm to rt and was extracted with EtOAc (3 x 100 mL). The combined organic layers were washed with brine, dried (Na2SO4), and concentrated to dryness. The crude residue was purified by ISCO chromatography using a gradient of 50 to 75% ethyl acetate in hexanes to afford 2.77 g (71%) of the desired product. ES-MS m/z 334.08 [M+H]+, HPLC RT (min) 0.97.

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 937046-98-5.

Reference:
Patent; BAYER PHARMACEUTICALS CORPORATION; WO2007/56170; (2007); A2;,
Bromide – Wikipedia,
bromide – Wiktionary