反应详情

11 g (0.05 mol) of N-(2-methyl-6-ethylphenyl)amino-tetrahydrofuran-2-one and 4.7 g (0.05 mol) of ammonium thioacetate are stirred in 80 ml of dimethylsulfoxide at 90° to 100° C. After cooling, the solution is poured into ice-water and extracted with methylene chloride. The combined extracts are repeatedly washed with water, dried over sodium sulfate and filtered and the filtrate is concentrated. Distillation of the residue under a high vacuum yields 5.7 g (48.5% of theory) of colourless N-(2-methyl-6-ethylphenyl)-amino-tetrahydrothiophen-2-one. Boiling point 167°-173° C. under 0.5 mm Hg.

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