반응 #3500

반응 방정식

water

sodium hydride

N-methoxy-p-chlorobenzamide

propargyl bromide

→

N-methoxy-N-propargyl-p-chlorobenzamide

수율 36.5%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   온도in this order while being cooled with ice
2. 2
   온도The mixture was heat-refluxed for 8 hours
3. 3
   workup.ADDITIONwas added to the reaction solution
4. 4
   추출the mixture was extracted with ethyl acetate
5. 5
   기타The extract was dried
6. 6
   농축concentrated
7. 7
   기타purified by silica gel column chromatography

실험 절차

0.22 g of sodium hydride (60% in oil) was suspended in 10 ml of tetrahydrofuran, and 1.0 g of N-methoxy-p-chlorobenzamide and 0.68 g of propargyl bromide were added thereto in this order while being cooled with ice. The mixture was heat-refluxed for 8 hours. After completion of the reaction, water was added to the reaction solution, and the mixture was extracted with ethyl acetate. The extract was dried, concentrated and purified by silica gel column chromatography to obtain 0.44 g of N-methoxy-N-propargyl-p-chlorobenzamide.

출처