反应详情

温度

50 °C

A mixture of 4-methylanthranilonitrile (4.46 g) and freshly fused zinc chloride (6.8 g) in 20 ml of nitrobenzene was heated at 50° C. for 1 hour. To this was added tetrahydrothiopyran-4-one (5.1 g) and the mixture was heated to 130° C. for 1.5 hours. After cooling, the zinc complex was filtered, rinsed with ethyl ether and partitioned between 2-butanone (MEK) and NH4OH. The aqueous phase was extracted with MEK and the organics were washed with water and dried (saturated NaCl, MgSO4). This was concentrated to give 4.76 g of an off-white powder, m.p. 239°-245° C. d., which was recrystallized from ethyl acetate to give 2.95 g of an off-white powder, m.p. 243°-246° C. d.

1. temperaturethe mixture was heated to 130° C. for 1.5 hours
2. temperatureAfter cooling
3. filtrationthe zinc complex was filtered
4. washrinsed with ethyl ether
5. custompartitioned between 2-butanone (MEK) and NH4OH
6. extractionThe aqueous phase was extracted with MEK
7. washthe organics were washed with water
8. dry with materialdried (saturated NaCl, MgSO4)
9. concentrationThis was concentrated