Tag: M.W=200-300

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 4766-33-0 as follows. Safety of 5-Bromonaphthalen-1-amine

General procedure: To a stirred solution of 3-chloro-6-nitrobenzo[d]isothiazole 1,1-dioxide (2) 1 mmol) in THF (15 mL), triethylamine (3 mmol) and aromatic amine (1 mmol) were added. The mixture was stirred at room temperature for 4~6 h. The solvent was eliminated in vacuo and the resulting residual was recrystallised from ethyl acetate/hexane to give the title compounds in mediate to high over yield.

According to the analysis of related databases, 4766-33-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Shang, Erchang; Wu, Yiran; Liu, Pei; Liu, Ying; Zhu, Wei; Deng, Xiaobing; He, Chong; He, Shan; Li, Cong; Lai, Luhua; Bioorganic and Medicinal Chemistry Letters; vol. 24; 12; (2014); p. 2764 – 2767;,
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. 68322-84-9, name is 2-Bromo-1-fluoro-4-(trifluoromethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., Formula: C7H3BrF4

Example 63 3- {2-Ethyl-4- [3-methyl-5- (2-o-tolyloxy-4-trifluoromethyl-phenoxy)-phenoxy]-phenyl}- propionic acid Step A A mixture 3-benzyloxy-5-methyl-phenol (8.50 g, 39.7 mmol), 3-bromo-4- fluorobenzotrifluoride (9.64 g, 39.7 mmol) and 325 mesh potassium carbonate (6.58 g, 47.6 mmol) in dry DMSO (100 mL) is heated to 100 C and stirred for 8 hours under N2. The reaction is cooled and acidified with 1 N HCI. The mixture is then diluted with water and extracted with Et20. The organic layer is dried (Na2S04), and the solvent is removed in vacuo to afford crude product that is absorbed on silica gel and purified by flash chromatography using 9/1 hexanes/ethyl acetate to afford 14.14 g (81%) product. Rf = 0.52 (4/1 hexanes/EtOAc).’H NMR (400 MHz, CDCl3).

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 68322-84-9.

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/37763; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 141474-37-5,Some common heterocyclic compound, 141474-37-5, name is 2,4-Dibromo-6-fluoroaniline, molecular formula is C6H4Br2FN, 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.

In a 1L round bottom flask, 2,4-dibromo-6-fluoroaniline 30 g (111.56 mmol), phenylboronic acid-d5 31.2 g (245.44 mmol), potassium carbonate (K2CO3) 61.9 g (446.27 mmol), tetrakis Triphenylphosphine palladium (Pd(PPh3)4) 2.6 g (2.20 mmol), water 120 mL, toluene 300 mL and tetrahydrofuran 300 mL was added and refluxed for 24 hours. When the reaction was completed, the resultant product was layer-separated to remove the aqueous layer, the organic layer was separated and concentrated under reduced pressure, and then the solid obtained by separation by column chromatography using hexane and dichloromethane as a development solvent was dried, yielding 24.2 g. 79.4% of a white solid was obtained.

The synthetic route of 141474-37-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SFC Ltd.; Lee Sang-hae; Sim So-yeong; Ryu Se-jin; (30 pag.)KR102121582; (2020); B1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 49764-63-8, name is 4,5-Dibromobenzene-1,2-diamine, 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 49764-63-8, Recommanded Product: 49764-63-8

Add to a pre-dried 100ml two-necked bottle, Triphenylamine 4-boronic acid (773mg),4,5-Dibromo-o-diaminobenzene (138 mg), Pd(PPh3)2Cl2 (40 mg), K2CO3 (424 mg). After nitrogen protection, 30 ml of toluene and 2 ml of deionized water were added, the temperature was raised to 80 C, and the reaction was carried out for 24 hours. After the reaction, the mixture was washed and extracted with dichloromethane and water several times. The organic phase was collected, dried over anhydrous magnesium sulfate, concentrated under reduced pressure, and then purified by column chromatography. 200-300 mesh silica gel was used as a stationary phase, and a dichloromethane / petroleum ether volume ratio 3: 1 mixture was used as a mobile phase to elute. The eluate containing the target compound was collected, and the solvent was distilled off under reduced pressure and dried. 488 mg of pink solid was obtained by thin layer chromatography with a yield of 82%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4,5-Dibromobenzene-1,2-diamine, and friends who are interested can also refer to it.

Reference:
Patent; Zhejiang University of Technology; Li Weijun; Xu Ning; Chen Zhangxin; Zhang Cheng; (14 pag.)CN110713493; (2020); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 4263-52-9, These common heterocyclic compound, 4263-52-9, name is Sodium 2-bromoethanesulphonate, 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 reactor was charged with 54.89 g (0.186 mol) methyloleate, 9.55 g (0.093 mol) diethylenetriamine and heated under an argon atmosphere with stirring to 160 C., whereupon methanol began to reflux, enough methanol was distilled off to bring to 180 C., stirring with argon sparging was continued for 2 days to yield pure 3-(2-((z)-hepatadec-8-en- 1 -y-1 -(2-oleamido ethyl)-4,5-dihydro- 1H-imidazoline as a viscous light straw colored fluid. ?3C NMR (ppm in CDC13, 100 MHz) oe=25.8, 36.6, 38.0, 46.6, 50.2, 52.2, 167.5, 173.4. A flask was charged with 4.000 g (6.514 mmol) 3-(2-((z)-hepatadec-8-en-1-yl)-1-(2-oleamido ethyl)-4,5-dihydro-1H-imidazoline, 1.648 g (7.810 mmol) sodium 2-bromoethylsulfonate, 20 ml anhydrous N-Methyl-2-pyrrolidone (NMP), heated under an argon atmosphere with stirring at 140 C. for 2 days. Evaporated the mixture in vacuo (90 C./0.8 mmHg), poured into 30 mL sodium chloride saturated deionized water, extracted with 20 mL aliquots of chloroform until the chloroform layer had only a faint color, combined the chloroform layer and dried over anhydrous magnesium sulfate, filtered through celite, vacuum distilled. A viscous dark amber fluid comprised of about 38 wt % of 2-(2-((Z)-heptadec-8-en-1-yl)-1-(2-oleamidoethyl)-4,5-dihydro-1H-imidazol-3-ium-3-yl)ethane-1-sulfonate (z-Im-1), 48 wt % Im and 15 wt % of NMP was obtained. The product was purified using flash chromatography with MeOH-water (9:1), and yield 80 mol % of z-IM-1. 13C NMR (ppm in CDCl3, 100 MHz) delta=170.8, 46.7, 47.4, 36.0, 46.3, 174.8, 25.7, 43.4, 45.7, 362, 25.6.

Statistics shows that Sodium 2-bromoethanesulphonate is playing an increasingly important role. we look forward to future research findings about 4263-52-9.

Reference:
Patent; GPCP IP Holdings LLC; Chen, Yu; Holtman, Kevin M.; Hammes, Brian S.; Boettcher, Jeffrey J.; (31 pag.)US2018/202109; (2018); 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. 3875-78-3, name is 6-Bromochroman belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C9H9BrO

To a mixture of 6-bromochroman (500 mg, 2.35 mmol, 1.30 equiv) in tetrahydrofuran (10 mL) was added n-BuLi (0.94 mL, 1.30 equiv, 2.5N) at -78 C. The mixture was stirred for 30 min at -78 C. After that was added a solution of 7-bromo-4-methoxy-2,3-dihydrobenzofuran-5-carbaldehyde (465 mg, 1.81 mmol, 1.00 equiv) in tetrahydrofuran (5 mL) at -78 C. The reaction was stirred at -78 C. for 1 h. NH4Cl/H2O was added and the mixture was extracted with EtOAc thrice. The combined extracts were washed with brine and dried over Na2SO4. The mixture was then concentrated and purified by chromatography on silica gel (3:1 PE/EA) to yield (7-bromo-4-methoxy-2,3-dihydrobenzofuran-5-yl)(chroman-6-yl)methanol as a yellow oil. MS (ES) m/z: 373[M-OH]+

The synthetic route of 3875-78-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Janssen Pharmaceutica NV; Xu, Guozhang; Kuo, Gee-Hong; Gaul, Micheal; (68 pag.)US2019/55226; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 15378-31-1, 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. 15378-31-1, name is 3-Bromo-2-(bromomethyl)prop-1-ene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

6.3 g of KF are added at -15 C. under nitrogen and with stirring to a solution of 21.8 g of trifluoromethyl trifluoromethanesulfonate in 50 ml of dry N,N-dimethylacetamide (DMA) in a three-necked flask with dry-ice condenser, and the mixture is stirred at this temperature for 0.5 hour. Gaseous trifluoromethanesulfonyl fluoride and a DMA suspension of potassium trifluoromethanolate form. 21.4 g of the dibromide are metered into the suspension, and the mixture is stirred at 50-60 C. for 24 hours. In order to isolate the product, the reaction mixture is cooled to room temperature and added to ice. The organic phase is separated off at 0 C., and the remaining phase is distilled at atmospheric pressure. A colourless, mobile liquid forms.

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-2-(bromomethyl)prop-1-ene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK PATENT GESELLSCHAFT MIT DESCHRANKTER HAFTUNG; US2011/82312; (2011); 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. 454-65-9, name is 3-Bromobenzene-1-sulfonyl fluoride, A new synthetic method of this compound is introduced below., Recommanded Product: 454-65-9

General procedure: To a Schlenk tube equipped with a stirrer, 4-biphenylsulfonyl fluoride (23.6 mg, 0.10 mmol) was added at room temperature,Tris (trimethylsilyl) amine (70.1 mg, 0.30 mmol, 1.5 equiv.) In DMF (0.50 mL) was charged,After cooling to 0 C.,P4-tBu base (37.5 muL, 0.030 mmol, 0.30 equiv.) Was added thereto.Trifluoromethane (excess) was then bubbled through for 1 minute After that, the reaction was carried out at the same temperature for 7 hours.After completion of the reaction, a saturated ammonium chloride aqueous solution was added,The organic layer was extracted with methylene chloride, the obtained organic layer was washed with a saturated sodium chloride aqueous solution,After drying over thorium, the solvent was distilled off under reduced pressure to obtain a crude product. The obtained crude product was purified by silica gel chromatography Purification by column chromatography gave 4- (trifluoromethylsulfonyl) biphenyl (3) as a target product in a yield of 84%.

The synthetic route of 454-65-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NAGOYA INSTITUTE OF TECHNOLOGY; TOSOH F-TECH INCORPORATED; SHIBATA, NORIO; OKUSU, SATOSHI; KAGAWA, TAKUMI; (11 pag.)JP2016/204275; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 57946-63-1, 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. 57946-63-1, name is 2-Bromo-4-(trifluoromethyl)aniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Heat a mixture of copper [(1)] cyanide (2.24g, 25.00 mmol), and 2-bromo-4- trifluoromethyl-phenylamine [(5.] [0G,] 20.83 mmol from Avocado) in [ L-METHYL-2-] pyrrolidinone (20 ml) to [195 ¡ãC] for four hours. Dilute the reaction mixture with 100 ml of ethyl acetate and wash the dark solution twice with 28percent aqueous ammonium hydroxide, twice with saturated aqueous sodium chloride (brine) and twice with water. Collect the organic layer, dry over sodium sulfate and remove the solvent under reduced pressure. Purify the residue via flash chromatography eluting with a step gradient starting with hexanes and going to 70percent hexanes with 30percent ethyl acetate to obtain 1. [821G] (9.78 mmol, 47percent yield) the title compound as a green amorphous solid: Mass Spectrum (m/e): 187 (M+1).

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-Bromo-4-(trifluoromethyl)aniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ELI LILLY AND COMPANY; WO2004/14895; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 1000994-95-5, The chemical industry reduces the impact on the environment during synthesis 1000994-95-5, name is 1-Bromo-4-(1,1-difluoroethyl)benzene, I believe this compound will play a more active role in future production and life.

Reference Example 17-1 4-(1,1-Difluoroethyl)benzaldehyde To a solution of 1-bromo-4-(1,1-difluoroethyl)benzene (1.00 g) in tetrahydrofuran (10.0 mL), n-butyl lithium (2.69 mol/L, solution in n-hexane, 1.68 mL) was added at -80C and the mixture was stirred at that temperature for 5 minutes. Subsequently, N,N-dimethylformamide (0.522 mL) was added at -80C and after stirring the mixture at that temperature for 20 minutes, 2 mol/L hydrochloric acid (2.50 mL) was added. After bringing the reaction mixture to room temperature, two extractions were conducted with ethyl acetate and the combined organic layers were washed with water. After drying over anhydrous magnesium sulfate and the desiccant was removed by filtration; the filtrate was then concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate = 100:0-90:10) to give the titled compound as a colorless oil (510 mg). 1H NMR (300 MHz, CHLOROFORM-d) delta ppm 1.95 (t, J=18.2 Hz, 3 H) 7.64 – 7.73 (m, 2 H) 7.92 – 7.98 (m, 2 H) 10.07 (s, 1 H). MS EI posi: 170[M]+.

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-4-(1,1-difluoroethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Taisho Pharmaceutical Co., Ltd.; TAKAYAMA, Tetsuo; SHIBATA, Tsuyoshi; SHIOZAWA, Fumiyasu; KAWABE, Kenichi; SHIMIZU, Yuki; HAMADA, Makoto; HIRATATE, Akira; TAKAHASHI, Masato; USHIYAMA, Fumihito; OI, Takahiro; SHIRASAKI, Yoshihisa; MATSUDA, Daisuke; KOIZUMI, Chie; KATO, Sota; EP2881384; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary