Extracurricular laboratory: Synthetic route of 7787-70-4

As the rapid development of chemical substances, we look forward to future research findings about 7787-70-4

Copper(I) bromide, cas is 7787-70-4, it is a common heterocyclic compound, the copper-catalyst compound, its synthesis route is as follows.,7787-70-4

Cuprous iodide (0.198 g, 1.04 mmol)Adding to a solution of 3,4-bis(diphenylphosphino)-2,5-dimethylthiophene (dpmt) (0.500 g, 1.04 mmol) synthesized in Example 1 in 30 mL of CH2Cl2,The mixture was stirred at room temperature for 5 h. Filter the reaction mixture,The solvent was removed under reduced pressure to give a pale yellow powder.The powder was dissolved in dichloromethane and recrystallized to give 0.615 g of yellow crystals.That is, the complex 1 was found to have a yield of 88.1%.

As the rapid development of chemical substances, we look forward to future research findings about 7787-70-4

Reference£º
Patent; Hubei University; Liu Li; Wei Qiong; (15 pag.)CN108997382; (2018); A;,
Copper catalysis in organic synthesis – NCBI
Special Issue “Fundamentals and Applications of Copper-Based Catalysts”

 

New learning discoveries about 7787-70-4

The synthetic route of 7787-70-4 has been constantly updated, and we look forward to future research findings.

7787-70-4,7787-70-4, Copper(I) bromide is a copper-catalyst compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A mixture of CuBr (28.7mg, 0.2mmol) and dppp (82.5mg, 0.2mmol) with an excess of batho (66.5mg, 0.2mmol) were dissolved in CH2Cl2 (5mL) and CH3OH (5mL) solution, stirred at room temperature for 6h. The insoluble residues were removed by filtration, and the filtrate was evaporated slowly at room temperature to yield yellow crystalline products. Yield: 80%. Anal. Calc. for C53H50BrCuN2O2P2: C, 66.84; H, 5.29; N, 2.94. Found: C, 66.97; H, 5.15; N, 2.88%. IR (KBr disc, cm-1): 3378s, 3048w, 2858w, 2580w, 1616w, 1556m, 1515m, 1433s, 1414m, 1229m, 1026s, 998w, 767m, 740s, 698vs, 513s, 482m. 1H NMR (600MHz, CDCl3, 298K): delta 7.87-8.98 (d, 6H, batho CH), 7.56-7.68 (m, 10H, batho CH), 7.41-7.24 (m, 20H, dppp CH), 2.91-2.81 (m, 4H, CH2), 2.78-2.63 (m, 2H, CH2); 31P NMR (400MHz, CDCl3, 298K): -12.25, -14.84.

The synthetic route of 7787-70-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Yu, Xiao; Fan, Weiwei; Wang, Guo; Lin, Sen; Li, Zhongfeng; Liu, Min; Yang, Yuping; Xin, Xiulan; Jin, Qionghua; Polyhedron; vol. 157; (2019); p. 301 – 309;,
Copper catalysis in organic synthesis – NCBI
Special Issue “Fundamentals and Applications of Copper-Based Catalysts”

 

Brief introduction of 7787-70-4

7787-70-4 Copper(I) bromide 24593, acopper-catalyst compound, is more and more widely used in various fields.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.7787-70-4,Copper(I) bromide,as a common compound, the synthetic route is as follows.

7787-70-4, General procedure: A mixture of CuCl (19.6mg, 0.2mmol) and dppb (89.3mg, 0.2mmol) with an excess of batho (66.5mg, 0.2mmol) were dissolved in CH2Cl2 (5mL) and 17 CH3OH (5mL) solution, stirred at room temperature for 6h. The insoluble residues were removed by filtration, and the filtrate was evaporated slowly at room temperature to yield yellow crystalline products.

7787-70-4 Copper(I) bromide 24593, acopper-catalyst compound, is more and more widely used in various fields.

Reference£º
Article; Yu, Xiao; Fan, Weiwei; Wang, Guo; Lin, Sen; Li, Zhongfeng; Liu, Min; Yang, Yuping; Xin, Xiulan; Jin, Qionghua; Polyhedron; vol. 157; (2019); p. 301 – 309;,
Copper catalysis in organic synthesis – NCBI
Special Issue “Fundamentals and Applications of Copper-Based Catalysts”

 

Analyzing the synthesis route of 7787-70-4

7787-70-4 Copper(I) bromide 24593, acopper-catalyst compound, is more and more widely used in various fields.

7787-70-4, Copper(I) bromide is a copper-catalyst compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,7787-70-4

To a Schlenk flask containing deoxygenated absolute ethanol (50 mL) was added in the following order, the CuBr (0.19 mmol, 0.027 g) and the ligand (L) (0.38 mmol, 0.10 g). The resulting solution was stirred at room temperature for 14 h. The solution was concentrated and a white precipitate appeared. The solid obtained was filtered off, and washed with diethyl ether (5 mL) under anaerobic conditions and dried under vacuum. 5: (Yield. 82%). Anal. Calc. for C30H28CuN8O2 (596.14 amu): C, 53.30; H, 4.17; N, 16.57. Found: C, 53.56; H, 4.27; N, 16.46%. Conductivity (Omega-1 cm2 mol-1, 1.2 * 10-3 M in CH3OH): 90. IR: (KBr, cm-1): 3325 nu(O-H), 3075 nu(C-H)ar, 2941 nu(C-H)al, 1604-1566 (nu(C=C), nu(C=N))ar, 1464 (delta(C=C), delta(C=N))ar, 1098, 1086 delta(C-H)ar,ip, 765, 696 delta(C-H)ar,oop. 1H NMR: (DMSO-d6 solution, 250 MHz, 298 K) delta: 8.67/8.62 [1H/1H, d, 3J = 4.7 Hz, 3J = 4.8 Hz, Hortho/Hortho’], 8.52/8.08 [1H/1H, t, 3J = 7.3 Hz, 3J = 7.0 Hz, Hpara/Hpara’], 8.05/7.94 [1H/1H, d, 3J = 7.3 Hz, H4/H4′], 7.62 [1H, s, Hpz], 7.83/7.55 [1H/1H, m, Hmeta/Hmeta’], 4.54 [2H, t, 3J = 5.1 Hz, NCH2-CH2OH], 4.02 [2H, t, 3J = 5.1 Hz, NCH2-CH2OH], 4.02 [2H,t, 3J = 5.1 Hz, NCH2-CH2OH]. In this complex, the signal attributableto proton hydroxyl (OH) is not observed. 13C{1H] NMR:(DMSO-d6 solution, 63 MHz, 298 K) delta: 158.5/153.2 (Cortho/Cortho’),143.4/140.2 (Cpara/Cpara’), 129.3/127.2 (C4/C40), 126.1/123.4 (Cmeta/Cmeta’), 108.2 (Cpz), 64.5, (NCH2-CH2OH), 58.6 (NCH2-CH2OH)ppm. ESI(+)(m/z) (%) = 596 (100%) [Cu(L)2]+.

7787-70-4 Copper(I) bromide 24593, acopper-catalyst compound, is more and more widely used in various fields.

Reference£º
Article; Guerrero, Miguel; Calvet, Teresa; Font-Bardia, Merce; Pons, Josefina; Polyhedron; vol. 119; (2016); p. 555 – 562;,
Copper catalysis in organic synthesis – NCBI
Special Issue “Fundamentals and Applications of Copper-Based Catalysts”

 

Downstream synthetic route of 7787-70-4

The synthetic route of 7787-70-4 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.7787-70-4,Copper(I) bromide,as a common compound, the synthetic route is as follows.

7787-70-4, Complex 2 was obtained by a similar method as described for 1 using copper(I) bromide (0.032 g,0.22 mmol) in place of copper(I) iodide. Colorless crystals of 2 were obtained (Yield: 0.191 g, 90.3%). 1HNMR (400 M, CDCl3) delta: 7.51-7.36 (m, 22H, m,p-Ph + H3,H4-PC6H4-), 7.33-7.27 (m, 4H, H5,H6-PC6H4-),7.12-7.00 (m, 12H, o-Ph). 13C NMR (100 M, CDCl3) delta: 147.87, 147.67, 140.24, 140.16, 134.31, 134.17, 133.45,131.80, 131.07, 130.71, 130.14, 129.90, 128.93, 128.69, 127.93, 127.26 (Ar-C). 31P NMR (240 M, CDCl3) delta:-9.70 (s). Anal. Calcd for C48H38Cu2Br2P2: C, 59.83; H, 3.97. Found: C, 59.88; H, 3.97. MS (MALDI-TOF): m/zCalcd for [M-2Br-Cu + C24H19P]+, 739.1745, found 739.1747.

The synthetic route of 7787-70-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Qi, Lei; Li, Qian; Hong, Xiao; Liu, Li; Zhong, Xin-Xin; Chen, Qiao; Li, Fa-Bao; Liu, Qian; Qin, Hai-Mei; Wong, Wai-Yeung; Journal of Coordination Chemistry; vol. 69; 24; (2016); p. 3692 – 3702;,
Copper catalysis in organic synthesis – NCBI
Special Issue “Fundamentals and Applications of Copper-Based Catalysts”

 

Application of (S)-(1-Ethylpyrrolidin-2-yl)methanamine

As the rapid development of chemical substances, we look forward to future research findings about 7787-70-4

A common heterocyclic compound, the copper-catalyst compound, name is Copper(I) bromide,cas is 7787-70-4, mainly used in chemical industry, its synthesis route is as follows.,7787-70-4

General procedure: A mixture of CuCl (19.6mg, 0.2mmol) and dppb (89.3mg, 0.2mmol) with an excess of batho (66.5mg, 0.2mmol) were dissolved in CH2Cl2 (5mL) and 17 CH3OH (5mL) solution, stirred at room temperature for 6h. The insoluble residues were removed by filtration, and the filtrate was evaporated slowly at room temperature to yield yellow crystalline products.

As the rapid development of chemical substances, we look forward to future research findings about 7787-70-4

Reference£º
Article; Yu, Xiao; Fan, Weiwei; Wang, Guo; Lin, Sen; Li, Zhongfeng; Liu, Min; Yang, Yuping; Xin, Xiulan; Jin, Qionghua; Polyhedron; vol. 157; (2019); p. 301 – 309;,
Copper catalysis in organic synthesis – NCBI
Special Issue “Fundamentals and Applications of Copper-Based Catalysts”

 

Analyzing the synthesis route of 7787-70-4

7787-70-4 Copper(I) bromide 24593, acopper-catalyst compound, is more and more widely used in various fields.

7787-70-4,7787-70-4, Copper(I) bromide is a copper-catalyst compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: CuI (0.095 g, 0.05 mmol) and PPh3 (0.262 g, 0.10 mmol) in 10 ml of MeCN were stirred for 1 h at 80 C to get a clear solution. To the reaction mixture, a solution of Hnor (0.082 g, 0.05 mmol) in methanol (5 mL) was added dropwise and left on stirring for 4 h. Then the mixture was filtered, and a colorless clear solution was obtained, which was left for slow evaporation leading to crystallization at room temperature. After a few days white crystals were obtained that were suitable for a single-crystal X-ray diffraction analysis.

7787-70-4 Copper(I) bromide 24593, acopper-catalyst compound, is more and more widely used in various fields.

Reference£º
Article; Khan, Rais Ahmad; Dielmann, Fabian; Liu, Xue; Hahn, F. Ekkehardt; Al-Farhan, Khalid; Alsalme, Ali; Reedijk, Jan; Polyhedron; vol. 111; (2016); p. 173 – 178;,
Copper catalysis in organic synthesis – NCBI
Special Issue “Fundamentals and Applications of Copper-Based Catalysts”

 

Downstream synthetic route of 7787-70-4

The synthetic route of 7787-70-4 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.7787-70-4,Copper(I) bromide,as a common compound, the synthetic route is as follows.

7787-70-4, a. 2-(carboxy-5-nitro-phenyl)malonic acid dimethyl ester (2) A solution of 2-chloro-4-nitrobenzoic acid (75g, 372mmol) in dimethyl malonate (900mL) was sparged with nitrogen for 15 min. Sodium methoxide (48.3g, 894mmol) was added in one portion and the contents exothermed to 48C. Fifteen minutes later, copper (I) bromide (5.4g, 37mmol) was added in one portion and the contents heated to 70C for 24 hrs. The reaction was 70% complete by nmr, the contents heated to 85C for 5 hrs to completely consume the 2-chloro-4-nitrobenzoic. Water (900mL) was added to the cooled reaction followed by hexanes (900mL). The aqueous layer was separated, toluene (900mL) added, filtered through celite, and aqueous layer separated. Fresh toluene (1800mL) was added to the aqueous layer and the biphasic mixture acidified with 6N aqueous HCl (90mL). A white precipitate formed and the contents stirred for 18 hrs. The product was filtered off and dried to give a white solid (78.1g, 70%) mp=153C. 1H NMR (CD3)2SO delta 8.37 (d, J = 2 Hz, 1H), 8.30 (d, J = 1Hz, 2H), 5.82 (s, 1H), 3.83 (s, 6H). 13C NMR (CD3)2SO delta 168.0, 167.3, 149.4, 137.1, 135.8, 132.5, 125.4, 123.7, 54.5, 53.4. Anal. Calcd for C11H10NO8: C, 48.49; H, 3.73; N, 4.71. Found: C, 48.27; H, 3.72; N, 4.76.

The synthetic route of 7787-70-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; PFIZER INC.; EP1181954; (2002); A2;,
Copper catalysis in organic synthesis – NCBI
Special Issue “Fundamentals and Applications of Copper-Based Catalysts”

 

Downstream synthetic route of 7787-70-4

The synthetic route of 7787-70-4 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.7787-70-4,Copper(I) bromide,as a common compound, the synthetic route is as follows.

7787-70-4, A mixture of PLN(37.6 mg, 0.2 mmol) containing CH3ONa (11.8 mg, 0.22 mmol) andCuBr (22 mg, 0.2 mmol) in methanolic solution (10 mL) was refluxed for 2 h, followed by addition of 1,10-phenanthroline (36 mg,0.2 mmol) in methanol (10 mL). The mixture was stirred for another 30 min at room temperature to give a dark-red solution and then filtered.The filtrate was kept in air for a week, forming dark-red block crystals. The crystals were isolated, washed three times with distilled water and dried in a vacuum desiccator containing anhydrous CaCl2. Yield: 87.9 mg (81%). Anal. Calcd for C24H19BrCuN2O4 (542.86): C,53.10; H, 3.52 and N, 5.16. Found: C, 53.12; H, 3.53 and N, 5.17. IR(KBr, cm-1): 3500, 3041, 1986, 1837, 1628, 1590, 1568, 1510, 1418,1344, 1196, 1159, 1106, 993, 855, 773, 720, 672, 631, 551, 548, 528,468, 455, 430.

The synthetic route of 7787-70-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Gou, Yi; Zhang, Zhan; Qi, Jinxu; Liang, Shichu; Zhou, Zuping; Yang, Feng; Liang, Hong; Journal of Inorganic Biochemistry; vol. 153; (2015); p. 13 – 22;,
Copper catalysis in organic synthesis – NCBI
Special Issue “Fundamentals and Applications of Copper-Based Catalysts”

 

Downstream synthetic route of Copper(I) bromide

With the synthetic route has been constantly updated, we look forward to future research findings about Copper(I) bromide,belong copper-catalyst compound

As a common heterocyclic compound, it belongs to quinuclidine compound,Quinuclidine-4-carboxylic acid hydrochloride,40117-63-3,Molecular formula: C8H14ClNO442,mainly used in chemical industry, its synthesis route is as follows.,7787-70-4

a. 2-(carboxy-5-nitro-phenyl)malonic acid dimethyl ester (2) A solution of 2-chloro-4-nitrobenzoic acid (75 g, 372 mmol) in dimethyl malonate (900 mL) was sparged with nitrogen for 15 min. Sodium methoxide (48.3 g, 894 mmol) was added in one portion and the contents exothermed to 480 C. Fifteen minutes later, copper (I) bromide (5.4 g, 37 mmol) was added in one portion and the contents heated to 70 C. for 24 hrs. The reaction was 70% complete by nmr, the contents heated to 85 C. for 6 hrs to completely consume the 2-chloro-4-nitrobenzoic. Water (900 mL) was added to the cooled reaction followed by hexanes (900 mL). The aqueous layer was separated, toluene (900 mL) added, filtered through celite, and aqueous layer separated. Fresh toluene (1800 mL) was added to the aqueous layer and the biphasic mixture acidified with 6N aqueous HCl (90 mL). A white precipitate formed and the contents stirred for 18 hrs. The product was filtered off and dried to give a white soid (78.1 g, 70%) mp=153 C. 1 H NMR (CD3)2 SO delta 78.37 (d, J=2 Hz, 1H), 8.30 (d, J=1 Hz, 2H), 5.82 (s, 1H), (3.83 (s, 6H). 13 C NMR (CD3)2 SO delta 168.0, 167.3, 149.4, 137.1, 135.8, 132.5, 125.4, 123.7, 54.5, 53.4. Anal. Calcd for C11 H10 NO8: C, 48.49; H, 3.73; N, 4.71. Found: C, 48.27; H. 3.72; N, 4.76.

With the synthetic route has been constantly updated, we look forward to future research findings about Copper(I) bromide,belong copper-catalyst compound

Reference£º
Patent; Pfizer INc.; US5919795; (1999); A;,
Copper catalysis in organic synthesis – NCBI
Special Issue “Fundamentals and Applications of Copper-Based Catalysts”