反应详情

To a solution of 45.2 g (0.44 mole) of sulfur dichloride in 200 ml of methylene chloride cooled to -5° C. under a nitrogen atmosphere was added a solution made up of 50.9 g (0.4 mole) of n-butyl N-methylcarbamate, 44.5 g (0.44 mole) of triethylamine and 100 ml of methylene chloride. The addition took 2 hours while the temperature was maintained at -15° C. to 0° C. After stirring for 1 hour the mixture was filtered under a positive nitrogen atmosphere, and the filtrate was concentrated. Solid was removed by extracting the product with hexanes. After filtration the hexane solution was concentrated to give 57.3 g of n-butyl N-chlorothio-N-methylcarbamate.

1. additionwas added a solution
2. additionThe addition
3. temperaturewas maintained at -15° C. to 0° C
4. filtrationwas filtered under a positive nitrogen atmosphere
5. concentrationthe filtrate was concentrated
6. customSolid was removed
7. extractionby extracting the product with hexanes
8. filtrationAfter filtration the hexane solution
9. concentrationwas concentrated