Category: 18282-59-2

These common heterocyclic compound, 18282-59-2, name is 4-Bromo-1,2-dichlorobenzene, 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. Formula: C6H3BrCl2

Mg (1.93 g, 79.4 mmol) was suspended in Et2O (50 ml). A chip of I2 was added, then heated to 45° C. 3,4-dichlorobenzylchloride (5.50 ml, 39.7 mmol) in Et2O (50 ml) was added slowly and the mixture was stirred at 45° C. for 2 h, then cooled to 23° C. In a second flask, CuCN (71 mg, 0.79 mmol) was suspended in Et2O (20 ml), then cooled to -30° C. under N2. The Grignard reagent was cannulated into the second flask, then warmed to -15° C. Compound 70 (4.75 g, 7.94 mmol) in Et2O (50 mL) was added dropwise. The mixture was stirred at -15° C. overnight, then warmed to 23° C. and stirred for 24 h. The reaction was quenched with 25percent aqueous sodium citrate at 0° C. and the product extracted with EtOAc. The combined organic extracts were washed with brine, dried (Na2SO4), filtered, and concentrated. Purification by silica gel chromatography (eluant: 3percent to 6percent EtOAc:hexane) gave 3.73 g (4.9 mmol, 62percent) of the product 71. MS (M+1): 759.

The synthetic route of 4-Bromo-1,2-dichlorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SCHERING CORPORATION; US2005/182095; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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 18282-59-2 as follows. Quality Control of 4-Bromo-1,2-dichlorobenzene

A. 1-Bromo-4,5-dichloro-2-nitro-benzene. 4-Bromo-1,2-dichlorobenzene (10.5 g, 46.3 mmol) was added to 25 mL concentrated sulfuric acid at 0° C. A 1:1 mixture of 70percent nitric acid and concentrated sulfuric acid (20 mL) was added dropwise over 40 min. The reaction mixture was allowed to warm to ambient temperature with stirring over 0.5 h, then was poured onto cracked ice. The resulting mixture was filtered through paper, and the collected solids were washed with water (5*) and then dried at 45° C. under reduced pressure for 30 min to provide 10.7 g of an 88:12 mixture of desired nitroarene to starting material. Recrystalization from absolute ethanol provided 4.76 g of long yellow needles corresponding to a 20:1 mixture of product to starting material. The mother liquor was concentrated and recrystallized twice to provide an additional 1.18 g of product (17:1 mixture with recovered starting material). TLC (silica gel, 1:1 hexanes/EtOAc): Rf=0.45. 1H NMR (400 MHz, CDCl3): 7.95 (s, 1H), 7.80 (s, 1H).

According to the analysis of related databases, 18282-59-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Allison, Brett; McAtee, Laura C.; Phuong, Victor K.; Rabinowitz, Michael H.; Shankley, Nigel P.; US2004/224983; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 18282-59-2, These common heterocyclic compound, 18282-59-2, name is 4-Bromo-1,2-dichlorobenzene, 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.

Method C; (3,4-Dichloro-phenyl) -(2,2,6,6-tetramethyl-piperidin-4-yl)-amine hydrochloric acid salt; A mixture of 4-amino-2,2,6,6-tetramethylpiperidine (3.4 ml, 20 mmol), potassium tert- butoxide (4.5 g, 40 mmol), 3,4-dichlorobromobenzene (4.97 g, 22 mmol), palladacycle (100 mg, 0.11 mmol) and dioxane (100 ml) was stirred at reflux for 2 h. Water (100 ml) was added and the mixture was extracted with diethyl ether (2 x 50 ml). Chromatography on silica gel with dichloromethane, methanol and conc. ammonia (89:10:1) gave the title compound. Yield 5.56 g, (82 percent). Hydrochloric acid in ether (6.5 ml, 3.1 M) was added and the hydrochloric acid salt was precipitated and stirred for 10 min, followed by filtration. Mp >300°C.

The synthetic route of 18282-59-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NeuroSearch A/S; WO2005/123679; (2005); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 18282-59-2, A common heterocyclic compound, 18282-59-2, name is 4-Bromo-1,2-dichlorobenzene, molecular formula is C6H3BrCl2, 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.

Tris [(DIBENZYLIDINEACETONE)] di palladium (0) (5 molpercent ; 23 mg) was added to a mixture of 1- [[4- (3-PIPERIDIN-1-YL-PROPOXY)-PHENYL]-PIPERAZINE (D11)] (150 mg; 0.49 [MMOL),] 3, 4-dichloro bromo benzene (160 mg; 1.2 eq), sodium [TERT-BUTOXIDE] (71 mg; 1.1 eq) and racemic 2,2′- bis (diphenylphosphino)-1, 1′-binaphthyl (7.5 molpercent ; 24 mg) in dry [TOLUENE] [(3ML).] The resulting mixture was heated at reflux under argon for 18 hours. The reaction was allowed to cool to room temperature and diluted with ethyl acetate (10 ml). The resulting solids were removed by filtration and the filtrate evaporated in vacuo. The residue was purified by column chromatography on silica eluting with 3percent methanol in [DICHLOROMETHANE] to afford the title compound as a buff solid (45 mg) MS (ES+) [M/E] 448 [M+H] +.

The synthetic route of 18282-59-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2004/35556; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 18282-59-2, name is 4-Bromo-1,2-dichlorobenzene, 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. Formula: C6H3BrCl2

Mg (1.93 g, 79.4 mmol) was suspended in Et2O (50 ml). A chip of I2 was added, then heated to 45° C. 3,4-dichlorobenzylchloride (5.50 ml, 39.7 mmol) in Et2O (50 ml) was added slowly and the mixture was stirred at 45° C. for 2 h, then cooled to 23° C. In a second flask, CuCN (71 mg, 0.79 mmol) was suspended in Et2O (20 ml), then cooled to -30° C. under N2. The Grignard reagent was cannulated into the second flask, then warmed to -15° C. Compound 70 (4.75 g, 7.94 mmol) in Et2O (50 mL) was added dropwise. The mixture was stirred at -15° C. overnight, then warmed to 23° C. and stirred for 24 h. The reaction was quenched with 25percent aqueous sodium citrate at 0° C. and the product extracted with EtOAc. The combined organic extracts were washed with brine, dried (Na2SO4), filtered, and concentrated. Purification by silica gel chromatography (eluant: 3percent to 6percent EtOAc:hexane) gave 3.73 g (4.9 mmol, 62percent) of the product 71. MS (M+1): 759.

The synthetic route of 4-Bromo-1,2-dichlorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SCHERING CORPORATION; US2005/182095; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 18282-59-2, name is 4-Bromo-1,2-dichlorobenzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 18282-59-2

A solution of 1-bromo-3,4-dichlorobenzene (16.92 g, 0.074 mol) in Et2O (100 ml) was added to a suspension of magnesium turnings in Et2O (60 ml) and the mixture was refluxed for 1 hour. The reaction was cooled to 23¡ã C. and a solution of 4-cyanopyridine 54 (7.80 g, 0.075 mol) in 1:1 Et2O:THF (150 ml) was added rapidly with vigorous stirring. The mixture was refluxed for 24 h, then cooled to 23¡ã C. Ice (100 g) was added, followed by 50percent H2SO4 (50 ml), and the mixture was stirred for 1 h. Et2O (100 ml) was added, the aqueous layer was separated, made basic with 10percent NaOH, and extracted with EtOAc (2.x.250 ml). The combined organic layer was dried (Na2SO4), filtered, and concentrated. Purification by silica gel chromatography (eluant: 30percent EtOAc: CH2Cl2) gave 12 g (0.047 mol, 64percent) of the product 55 as a colorless oil. MS (FAB for M+1): m/e 252.

According to the analysis of related databases, 18282-59-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SCHERING CORPORATION; US2005/182095; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics