반응 #1972790

반응 방정식

3,4-dimethylbenzenethiol

2-methyleneglutaronitrile

→

2-(3,4-dimethylphenylthiomethyl)glutaronitrile

용매

ethanol

ethanol

반응 조건

후처리

1. 1
   온도was refluxed for 5 hours
2. 2
   농축After the reaction mixture was concentrated in vacuo
3. 3
   workup.DISSOLUTIONthe resulting residue was dissolved in chloroform
4. 4
   세척washed with water
5. 5
   건조dried over MgSO4
6. 6
   기타The solvent was evaporated at reduced pressure
7. 7
   기타the residue was purified by flash column chromatography on silica
8. 8
   세척by eluting with benzene/ethyl acetate (7:1)

실험 절차

A mixture of 3,4-dimethylbenzenethiol (0.59 ml), 2-methyleneglutaronitrile (0.48 ml), ethanol (10 ml), and triton B (40% ethanol solution, 5 drops) was refluxed for 5 hours. After the reaction mixture was concentrated in vacuo, the resulting residue was dissolved in chloroform, washed with water, and dried over MgSO4. The solvent was evaporated at reduced pressure, and the residue was purified by flash column chromatography on silica by eluting with benzene/ethyl acetate (7:1) to give 1.18 g of 2-(3,4-dimethylphenylthiomethyl)glutaronitrile as an oil.

출처