反应详情

A solution of methylisothiocyanate (0.21 g.) in acetone (10 ml.) was added to a solution of trifluoromethanesulphonamide (0.45 g.) and sodium hydroxide (0.12 g.) in water (5 ml.), the mixture stirred at 60° for 18 hours and then evaporated to dryness. The residue was dissolved in water and the solution washed with ethyl acetate and then adjusted to pH 1 with concentrated hydrochloric acid. The mixture was treated with charcoal and filtered and the filtrate extracted with ethyl acetate. The combined ethyl acetate extracts were dried and evaporated to dryness and the residue recrystallised from petroleum ether (b.p. 60°-80°) to give 1-methyl-3-trifluoromethanesulphonylthiourea (0.27 g.), m.p. 88°-90°.

1. customevaporated to dryness
2. dissolutionThe residue was dissolved in water
3. washthe solution washed with ethyl acetate
4. additionThe mixture was treated with charcoal
5. filtrationfiltered
6. extractionthe filtrate extracted with ethyl acetate
7. dry with materialThe combined ethyl acetate extracts were dried
8. customevaporated to dryness
9. customthe residue recrystallised from petroleum ether (b.p. 60°-80°)