反应详情

13.65 g (0.1 m) of 3-chloro-3-acetylpropanol (b.p. 90°-110° C/2 mmHG; nD20 1.4740) prepared according to the method described by J. R. Stevens and G. A. Stein, J. Am. Chem. Soc. 62, 1045 (1940), were refluxed with 18.6 g (0.15 m) potassium thiolacetate in 100 ml of acetone for about 2 hours. After cooling the reaction mixture was filtered and the filtrate evaporated to dryness and the residue dissolved in water. The aqueous solution was extracted five times with chloroform and the combined extracts washed, dried and evaporated. Distillation of the residue yielded 3-thioacetoxy-2-methyl-4,5-dihydrofuran, b.p. 57°-59° C/0.6 mmHg.

1. temperatureAfter cooling the reaction mixture
2. filtrationwas filtered
3. customthe filtrate evaporated to dryness
4. dissolutionthe residue dissolved in water
5. extractionThe aqueous solution was extracted five times with chloroform
6. washthe combined extracts washed
7. customdried
8. customevaporated
9. distillationDistillation of the residue