反应详情

A mixture of 99.7 g (0.85 mol) of ethyl oxamate and 552 g (4.23 mol) of chlorocarbonylsulfenyl chloride, prepared in accordance with British Pat. No. 1,079,348, in toluene was held at reflux for 5.25 hours and then was concentrated under vacuum. Benzene was added to the residue, and the solution was extracted twice with water, twice with 5% NaHCO3, again with water, and was dried (CaSO4) and concentrated under vacuum. The residual oil was filtered to remove sulfur and was crystallized twice from methylcyclohexane to give 95.61 g (64%) of white solid, mp 49°-50.5 C.

1. customprepared in accordance with British Pat
2. temperatureat reflux for 5.25 hours
3. concentrationwas concentrated under vacuum
4. additionBenzene was added to the residue
5. extractionthe solution was extracted twice with water, twice with 5% NaHCO3, again with water
6. dry with materialwas dried (CaSO4)
7. concentrationconcentrated under vacuum
8. filtrationThe residual oil was filtered
9. customto remove sulfur
10. customwas crystallized twice from methylcyclohexane