反应详情

温度

150 °C

11 g (0.05 mol) of N-(2-methyl-6-ethylphenyl)amino-tetrahydrofuran-2-one and 6.6 g (0.05 mol) of potassium thioacetate are dissolved in 200 ml of diethylene glycol dimethyl ether and the solution is stirred for 20 hours at 150° C. After cooling, the mixture is poured into ice-water and extracted with methylene chloride. The combined extracts are washed repeatedly with water, dried over sodium sulfate and filtered and the filtrate is concentrated. After distillation under a high vacuum, the residue yields 5.2 g (44.2% of theory) of N-(2-methyl-6-ethylphenyl)-amino-tetrahydrothiophen-2-one. Boiling point 160°-165° C. under 0.45 mm Hg.

1. temperatureAfter cooling
2. extractionextracted with methylene chloride
3. washThe combined extracts are washed repeatedly with water
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationthe filtrate is concentrated
7. distillationAfter distillation under a high vacuum