反应 #63525

反应方程式

ethyl acetate

N-methylcyclohexylamine

4-chlorobutyryl chloride

triethylamine

→

N-methyl-N-cyclohexyl-4-chlorobutyramide

溶剂

water

反应条件

后处理

1. 1
   其他at 10° to 20° C.
2. 2
   温度cooling
3. 3
   workup.ADDITIONis added to the reaction mixture
4. 4
   其他The organic layer is separated
5. 5
   洗涤washed with water an aqueious saturated potassium carbonate solution, 10% aqueous hydrochloric acid and water in order
6. 6
   干燥dried over anhydrous sodium sulfate
7. 7
   过滤After filtering off sodium sulfate
8. 8
   浓缩the mother liquor is concentrated
9. 9
   workup.DISTILLATIONdistilled under reduced pressure

实验过程

To ethyl acetate (400 ml) is added N-methylcyclohexylamine (26 ml), and to the mixture are added dropwise with stirring 4-chlorobutyryl chloride (25 ml) and triethylamine (33.5 ml) over a period of 20 minutes with keeping the inner temperature at 10° to 20° C. by ice-cooling. The mixture is further stirred at room temperature for one hour. After the reaction, water is added to the reaction mixture. The organic layer is separated and washed with water an aqueious saturated potassium carbonate solution, 10% aqueous hydrochloric acid and water in order, and then dried over anhydrous sodium sulfate. After filtering off sodium sulfate, the mother liquor is concentrated and distilled under reduced pressure to give N-methyl-N-cyclohexyl-4-chlorobutyramide (41.5 g), b.p. 133°-136° C./2 mmHg.

来源