反应详情

2-Nitro-4-trifluoromethylbenzonitrile (10.8 g) and potassium carbonate (8.3 g) were heated to reflux in acetonitrile. A solution of 1-methylpropanethiol (5 g) in acetonitrile was added. The resultant suspension was heated at reflux for 4.5 hours. After cooling water was added and the mixture extracted with ethyl acetate. The organic extracts were washed with water. The organic extracts were washed with water, dried (anhydrous magnesium sulphate) and filtered. The filtrate was evaporated to dryness and the residue purified by column chromatography eluting with ethyl acetate in cyclohexane to give 2-(1-methylpropylsulphenyl)-4-trifluoromethylbenzonitrile (9.7 g) as a yellow oil, NMR (CDCl3) 1.0(t,3H), 1.2(d,3H), 1.5(m,1H), 3.4(m,1H), 7.3(m,1H), 7.6(m,2H).

1. temperatureat reflux for 4.5 hours
2. additionwas added
3. extractionthe mixture extracted with ethyl acetate
4. washThe organic extracts were washed with water
5. washThe organic extracts were washed with water
6. dry with materialdried (anhydrous magnesium sulphate)
7. filtrationfiltered
8. customThe filtrate was evaporated to dryness
9. customthe residue purified by column chromatography
10. washeluting with ethyl acetate in cyclohexane