반응 #55079

반응 방정식

sodium carbonate

NaOH

chloroacetic acid

HCl

3,4-dichlorobenzylchloride

thiourea

→

stated product

수율 89.3%

3,4-Dichlorobenzylthioacetic acid

수율 89.3%

용매

water

water

water

반응 조건

후처리

1. 1
   온도are heated
2. 2
   온도under reflux for 30 minutes
3. 3
   기타is run in at 60°-70° C.
4. 4
   온도the mixture is heated
5. 5
   온도under reflux for 15 minutes
6. 6
   기타is run in at 60°-70° C.
7. 7
   온도the mixture is maintained
8. 8
   온도under reflux for 1 hour
9. 9
   추출extracted with ether
10. 10
    세척the extract is washed with water
11. 11
    기타dried
12. 12
    기타evaporated
13. 13
    여과filtered off

실험 절차

A mixture of 19.5 g (0.1 mol) of 3,4-dichlorobenzylchloride and 7.6 g (0.1 mol) of thiourea in 50 ml of water are heated under reflux for 30 minutes with stirring, and then a solution of 16 g (0.4 mol) of NaOH in 25 ml of water is run in at 60°-70° C.; the mixture is heated under reflux for 15 minutes, a solution of 15 g (0.15 mol) of chloroacetic acid, 7 g of sodium carbonate and 50 ml of water is run in at 60°-70° C., and the mixture is maintained under reflux for 1 hour. The mixture is acidified cold with concentrated HCl, extracted with ether, and the extract is washed with water, dried and evaporated. The residue is taken up in petroleum ether and filtered off. 21 g of the stated product are obtained (yield: 83%) melting point: 63°-64° C.

출처