반응 #998465

반응 방정식

4-mercapto-benzonitrile

bromoethane

potassium carbonate

→

desired intermediate

수율 83.0%

4-Ethylthio-benzonitrile

수율 83.0%

용매

DMF

반응 조건

후처리

1. 1
   기타partition between brine (20 mL) and EtOAc (20 mL)
2. 2
   기타Separate the organic layer
3. 3
   건조dry over anhydrous Na2SO4
4. 4
   농축concentrate
5. 5
   기타Purify by chromatography on silica gel eluting with hexane/EtOAc (1:0, 9:1 and 4:1)

실험 절차

Combine 4-mercapto-benzonitrile (0.4 g, 2.96 mmol), bromoethane (1.4 mL, 8.88 mmol) and potassium carbonate (3.3 g, 23.7 mmol) in anhydrous DMF (7 mL) and heat at 60° C. for 17 h. Cool the reaction mixture to ambient temperature and partition between brine (20 mL) and EtOAc (20 mL). Separate the organic layer, dry over anhydrous Na2SO4 and concentrate. Purify by chromatography on silica gel eluting with hexane/EtOAc (1:0, 9:1 and 4:1) to obtain the desired intermediate as a colorless oil (0.4 g, 83%).

출처