1-Azepan-1-yl-2-chloro-ethanone synthesis

Yield:52227-33-5 100%

Reaction Conditions:

with triethylamine in dichloromethane at 5;Inert atmosphere;Large scale;

Steps:

Step 4, the synthesis of BAZ-B-1

S41: in a 20L kettle, under the condition of feeding nitrogen, put in 16.5L dichloromethane, 1018.6g hexamethyleneimine, 1200.0g triethylamine, and cool to 5°C;S42: the temperature is controlled at 5°C, 1100.0 g of chloroacetyl chloride is added dropwise, and the dropwise addition time is controlled to be 4-5h;S43: the dropwise addition is completed, and the reaction is incubated under the condition that the temperature is 5°C;S44: the reaction is completed, under the condition that the temperature is 5 , put into 1100mL saturated sodium bicarbonate solution, stir for 20min, stand for 30min, and separate the liquids to obtain the orange-yellow organic layer a and the water layer, and the water layer is discarded;S45: under the condition that the temperature is 5°C, put into the orange-yellow organic layer a and 3300 mL of saturated sodium chloride solution, stir for 20 minutes, let stand for 30 minutes, and separate the liquids to obtain the orange-yellow organic layer b and the water layer, and the water layer is discarded;S46: drop into the orange-yellow organic layer b, 550 g of anhydrous magnesium sulfate, stir for 30min, and filter with suction to obtain a wine-red solution;S46: Concentrate the wine red solution to a moisture content of less than 0.5% under the conditions that the temperature is below 50°C and the degree of vacuum is -0.08MPa to obtain 1950g of brown viscous liquid, which is BAZ-B-1, and the yield is 100%, the BAZ-B-1 is 1-azepan-1-yl-2-chloroethanone;

References:

CN113816892,2021,A Location in patent:Paragraph 0048; 0153-0160