反応 #63525

反応方程式

ethyl acetate

N-methylcyclohexylamine

4-chlorobutyryl chloride

triethylamine

→

N-methyl-N-cyclohexyl-4-chlorobutyramide

溶媒

water

反応条件

後処理

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

実験手順

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.

出典