Author: Jessica.F

Electric Literature of 4101-68-2,Some common heterocyclic compound, 4101-68-2, name is 1,10-Dibromodecan, molecular formula is C10H20Br2, 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.

To a suspension of phthalimide potassium salt (5.57 g, 30 mmol) and K2CO3 (15.00 g, 100 mmol) in CH3CN (100 mL) was added1,10-dibromodecane (49.94 g, 185 mmol), then the mixture was refluxed for 11 hours. The obtained mixture was filtered and CH3CN was removed by a rotary evaporator. The crude product was purified by column chromatography (SiO2, PE/EA = 6 : 1) to give a whitesolid (10.19 g, 93 %).

The synthetic route of 4101-68-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Mengjun; Du, Xusheng; Tian, Huasheng; Jia, Qiong; Deng, Rong; Cui, Yahan; Wang, Chunyu; Meguellati, Kamel; Chinese Chemical Letters; vol. 30; 2; (2019); p. 345 – 348;,
Bromide – Wikipedia,
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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. 591-19-5, name is 3-Bromoaniline, A new synthetic method of this compound is introduced below., HPLC of Formula: C6H6BrN

c. 3,4-Dibromoaniline. 3-Bromoaniline (3 g, 17.4 mmol) was dissolved in 15 ml CH2 Cl2 and the reaction mixture was cooled to -10 C. in an ice-salt bath. 2,4,4,6-Tetrabromo-2,5-cyclohexadienone, (9.29 g, 0.02 mmol) was added in small portions with constant stiting. The reaction mixture was stirred for a period of 7 hours at 0 C. after which the reaction was quenched with 2N NaOH (10 ml). The aqueous layer was extracted with CH2 Cl2 and the organic layer was dried over anhydrous Na2 SO4. The CH2 Cl2 layer was concentrated in vacuo and purified by column chromatography. Elution with 0-3% ethyl acetate/n-hexanes yielded 3.2 g (12.7 mmol, 73%) of pure product; mp 80-81 C.; IR (KBr) 3406, 3318, 3210, 1583, 1464, 1287, 1108, 860, 668; 1 H NMR (CDCl3) 6 6.49 (dd,1H,J=2.7,8.6), 6.7 (d,1H,J=2.64), 7.32 (d,1H,J=8.6); 13 C NMR (CDCl3) 6 112.6, 116, 120.1, 125.45, 134.26, 147.08.

The synthetic route of 591-19-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Rutgers, The State University of New Jersey; US6063801; (2000); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 103-64-0, A common heterocyclic compound, 103-64-0, name is (2-Bromovinyl)benzene, 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.

General procedure: A round-bottom flask was charged with phenylacetylene (0.75 mmol, 0.08 mL), K2CO3 (0.75 mmol, 100 mg), PEG 200 (1 mL), and aryl halide (0.5 mmol). To this mixture, Pd(0) nano-catalyst supported on SDPP (1.5 mol-%, 3.0 mg) prepared according to our previous report [13] was added. In the case of aryl iodides and activated aryl bromides, the reaction mixture was placed in a 100 C oil bath; and in the case of the less active and deactivated aryl bromides and chlorides, the reaction mixture was placed in a 120 C oil bath. After completion of the reaction, the catalyst was removed by centrifugation and the remaining mixture was extracted with ethyl acetate (310 mL) and water several times and dried over anhydrous Na2SO4. The organic layer was evaporated under reduced pressure, and then purified by column chromatography over silica gel 60 (230-240 mesh; Merck) using petroleum ether/ethyl acetate (5 : 1) as eluent to afford the product with high purity in 51-95% yield. Note: This procedure can also be used, but the catalyst is prepared in situ by adding the appropriate amounts of SDPP and Pd(OAc)2.

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:
Article; Iranpoor, Nasser; Firouzabadi, Habib; Motevalli, Somayeh; Rajabi, Khashayar; Australian Journal of Chemistry; vol. 68; 6; (2015); p. 926 – 930;,
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. 54962-75-3, name is 3-Bromo-5-(trifluoromethyl)aniline, This compound has unique chemical properties. The synthetic route is as follows., Safety of 3-Bromo-5-(trifluoromethyl)aniline

3-bromo-5-trifluoromethylaniline (48 g, 0.2 mol) was added to a three-necked flask equipped with argon,4-methylimidazole (19.7 g, 0.24 mol), cuprous iodide (5.7 g, 0.03 mol)8-hydroxyquinoline (4.4 g, 0.03 mol)(30g, 0.22mol) and 300ml of DMSO, stirred and heated to 120 C for 24 h, followed by TLC. After the reaction was completed, the mixture was cooled to 50 C. 200 ml of 14% aqueous ammonia was added and stirring was continued for 1 h. Water and ethyl acetate were extracted three times. The organic phases were combined, washed with saturated brine, dried over anhydrous magnesium sulfate, filtered and the solvent was removed by rotary distillation.Then, the solvent was cooled in a refrigerator, and the precipitated crystals were filtered and dried to obtain 33.7 g of pale green needle-like crystals in a yield of 70%.

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 54962-75-3.

Reference:
Patent; Zhejiang Dade Pharmaceutical Group Co., Ltd.; Wang Jianping; Wang Jianguo; (14 pag.)CN107226809; (2017); A;,
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. 615-59-8, name is 1,4-Dibromo-2-methylbenzene, A new synthetic method of this compound is introduced below., Product Details of 615-59-8

(1) 2,5-dibromotoluene (10 mmol, 2.5 g), 4-methoxycarbonylbenzeneboronic acid (24 mmol, 4.33 g) under N2 protection.caesium fluoride (40 mmol, 6.0 g) was placed in a 250 mL three-necked flask, and 5% (1.2 to 2.0 g) of Pd (PPh3) catalyst was added.100 mL of anhydrous THF was used as a solvent, and refluxed at 67 C.After completion of the reaction, the product was isolated by silica gel column chromatography (petroleum ether, dichloromethane) to give a pink solid 2.91 g, yield 81%.

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; Shandong Normal University; Dong Yubin; Wang Jiancheng; Liu Congxue; Hu Yuhong; (14 pag.)CN108640906; (2018); A;,
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. 58971-11-2, name is 3-Bromophenethylamine belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C8H10BrN

To a mixture of 2-(3-bromophenyl)ethanamine (485 mg, 2.42 mmol) and K2CO3 (469 mg, 3.39 mmol) in acetonitrile (7.3 mL) was added 1-bromo-2-methoxyethane (228 muL, 2.42 mmol), and the mixture was stirred ON at rt. The mixture was then heated at reflux for 6 h. An additional portion of 1-bromo-2-methoxyethane (75 muL, 0.80 mmol) was added, and heating was continued ON. The reaction mixture was filtered. The filtrate was concentrated, and residue purified by flash chromatography to provide 37A (189 mg, 30.2%). MS(ESI) m/z 257.9 (M+H).

The synthetic route of 58971-11-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; SMALLHEER, Joanne M.; KICK, Ellen K.; VALENTE, Meriah Neissel; HU, Carol Hui; HALPERN, Oz Scott; JUSUF, Sutjano; (133 pag.)WO2018/5336; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 10485-09-3, These common heterocyclic compound, 10485-09-3, name is 2-Bromoindene, 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.

(Comparative Example 3) 1.2 ml of a tetrahydrofuran solution of 0.25 g of magnesium was cooled to 0C, and 5.0 ml of a tetrahydrofuran solution of 1.0 g of 2-bromoindene was slowly dropped thereto.After the dropping, the mixture was stirred at the same temperature for 1 hour, and 0.57 g of 2,6- dimethylbenzaldehyde was added thereto, and stirred for 12 hours while the temperature was being raised to 25C.After the confirmation of the degree of reaction progress by TLC, the reaction was terminated with an ammonium chloride aqueous solution, and an organic phase was extracted with ethyl acetate.[0132] After the obtained organic phase was dried with anhydrous magnesium sulfate, the organic phase was concentrated and purified by column chromatography. Then, 5 g of manganese dioxide was added to 30 ml of a chloroform solution of the obtained intermediate compound, and the mixture was stirred at 25 C for 12 hours. After the confirmation of the degree of reaction progress by TLC, the manganese dioxide was filtered, and 0.42 g (yield: 40%) of Comparative Product 3 shown below was obtained by recrystallization. Thestructure of Comparative Product 3 was confirmed by 1HNMR. 1H-NMR (CDC13; TMS) : delta 2.21 (s, 6H) , 3.85 (s, 2H) , 7.07 (d, 2H) , 7.20-7.26 (m, 2H) , 7.33-7.41 (m, 2H) , 7.47 (d, 1H) , 7.58 (d, 1H)

The synthetic route of 10485-09-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CANON KABUSHIKI KAISHA; SAITOH, Terunobu; WO2011/81078; (2011); A1;,
Bromide – Wikipedia,
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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 4101-68-2 as follows. name: 1,10-Dibromodecan

2.2.4 9-(10-bromodecyl)-9H-carbazole (4) Under argon atmosphere, carbazole (1.67 g, 0.01 mol), anhydrous potassium carbonate (2.77 g, 0.02 mol), and 1,10-dibromodecane (6.00 g, 0.02 mol) in 40 mL of anhydrous acetonitrile were refluxed at 95 C for 36 h. After cooling to room temperature, insoluble substance was filtered, and the solvent was removed under reduced pressure. The crude product was purified by column chromatography on silica gel with petroleum to get 9-(10-bromodecyl)-9H-carbazole as white crystals (1.66 g, Yield 43%). 1H NMR (500 MHz, CDCl3, delta): 8.08 (d, J = 7.7 Hz, 2H, Ar-H), 7.43 (t, J = 7.8 Hz, 2H, Ar-H), 7.35 (d, J = 8.1 Hz, 2H, Ar-H), 7.20 (t, J = 7.5 Hz, 2H, Ar-H), 4.21 (t, J = 7.3 Hz, 2H, CH2), 3.33 (t, J = 6.8 Hz, 2H, CH2Br), 1.79 (m, 4H, CH2), 1.33-0.91 (m, 12H, CH2). FT-IR (cm-1, KBr): 2930, 2850 (s; CH), 1632, 1619, 1593 (m; Ar). Anal. Calcd. For C22H28BrN: C, 68.39; H, 7.30; N, 3.63; Found: C, 68.47; H, 7.25; N, 3.56.

According to the analysis of related databases, 4101-68-2, the application of this compound in the production field has become more and more popular.

Reference:
Article; Huang, Jin; Wang, Weina; Gu, Jiangjiang; Li, Weizhi; Zhang, Qiuhong; Ding, Yin; Xi, Kai; Zheng, Youxuan; Jia, Xudong; Polymer; vol. 55; 26; (2014); p. 6696 – 6707;,
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. 5433-01-2, name is 1-Bromo-3-isopropylbenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 5433-01-2

Preparation Example 1-1: Preparation of 4-t-butyl-N- (4- isopropylphenyl ) benzenamine; As represented below in Reaction Scheme 1, 25g of 3-t- butylaniline (0.125mol) and 37.3g of 3-bromoisopropylbenzene(0.25mol) were dissolved in 25OmL of toluene, and 3.43g ofPd2(dba)3 (0.0037mol) was added thereto under a nitrogen atmosphere. Then, 14.4g of NaOBufc (0.15mol) and 1.157g of (t- Bu)3P (0.0075mol) were added to the reaction solvent, and the reaction mixture was refluxed and stirred for 12 hours. The reaction mixture was checked for the completion of the reaction by means of TLC, and if the reaction was completed, the reaction product was cooled down to room temperature. The reacted solution was poured onto a thin silica pad to perform short chromatography, and then was washed with methylene chloride (MC) . The washed solution was subjected to distillation under reduced pressure to thereby remove the solvent, and was chromatographed using n-hexane to thereby obtain a desired white solid product (29.4g, 88%). [Reaction Scheme 1]

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; DOOSAN CORPORATION; WO2009/91095; (2009); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 51376-06-8, name is 5-Bromobenzo[c][1,2,5]oxadiazole, 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 51376-06-8, Computed Properties of C6H3BrN2O

5-bromo-2,1,3-benzoxadiazole (0.71 g), cesium carbonate (1.4 g), 2,2′- bis(diphenylphosphino)-1,r-binapthyl (0.17 g) and Tris-(dibenzylideneacetone) dipalladium(O) (0.13g) were added to a solution of (5S)-3-[3-fluoro-4-(piperidin-4- yloxy)phenyl]-5-[(isoxazol-3-ylamino)methyl]-1,3-oxazolidin-2-one (1.3 g) (obtained from Step b) in dry dimethylformamide (15 mL) and the reaction mixture was heated at 100 C for about 17 hours. The reaction mixture was filtered and the solvent was evaporated. The crude product thus obtained was purified by column chromatography using 1 % methanol in dichloromethane to yield the title product (0.07g).Melting point: 75-100 C; EIMS (m/z): 534.21; 1HNMR(DMSO): delta 8.16 (s, 1H), 7.66 (d, 1H), 7.48 (dd, 1H), 7.3 (m, 2H), 7.17 (d, 1H), 7.08-7.05 (t, 1H), 6.75 (s, 1H), 4.99 (m, 1H), 4.53 (m, 3H), 4.14-4.11 (t, 1H), 3.95 (t, 1H), 3.61 (m, 2H), 3.3 (m, 2H), 2.04 (m, 4H).

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, 5-Bromobenzo[c][1,2,5]oxadiazole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; RANBAXY LABORATORIES LIMITED; WO2006/35283; (2006); A1;,
Bromide – Wikipedia,
bromide – Wiktionary