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ChemicalBook CAS DataBase List 2-(BROMOACETYL)PYRIDINE HYDROBROMIDE
17570-98-8

2-(BROMOACETYL)PYRIDINE HYDROBROMIDE synthesis

3synthesis methods
2-Acetylpyridine

1122-62-9

2-(BROMOACETYL)PYRIDINE HYDROBROMIDE

17570-98-8

The general procedure for the synthesis of 2-bromo-1-(2-pyridyl)-1-acetone hydrobromide from 2-acetylpyridine was as follows: bromine (1.52 mL, 9.72 mmol) was slowly added dropwise to a 30% hydrobromide/acetic acid (12 mL) solution containing 2-acetylpyridine (3 g, 24.8 mmol) at 15 °C. After the dropwise addition was completed, the reaction mixture was warmed to 40 °C and kept stirring for 1 h. Subsequently, it was continued to be warmed to 75 °C and stirred for 1 h. The reaction mixture was then heated up to 40 °C and kept stirring for 1 h. Upon completion of the reaction, the reaction solution was cooled to 20 °C, ether (30 mL) was added and stirred at this temperature for 30 minutes. The resulting yellow precipitate was collected by filtration, and the precipitate was washed with ether (10 mL) and dried to afford the target product 2-bromo-1-(2-pyridyl)-1-acetone hydrobromide (6.81 g, 97.8% yield).

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Yield:17570-98-8 97.8%

Reaction Conditions:

with hydrogen bromide;bromine;glacial acetic acid at 15 - 75; for 2 h;

Steps:

1.1.3 (3) 2-Bromo-acetylpyridineHydrobromide (C)synthesis:

At 15 , the bromine (1.52mL, 9.72mmol) was slowly added dropwise to 2-acetyl-pyridine (3g, 2.78mmol) in 30% HBr / HOAc (12mL), and after completion of the dropwise addition, the reaction solution at 40 under stirring 1h, then stirred at 75 1h. The reaction solution was cooled to 20 , to which was added Et2O (30mL), and stirred at this temperature for 30min, the resulting yellow precipitate was filtered, and the precipitate was washed with 10mL diethyl ether, and dried to (6.81g, 97.8%).

References:

CN105524056,2016,A Location in patent:Paragraph 0048; 0049; 0050

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