反应详情

Powdered potassium hydroxide (2.5 g), 4.7 g. 10.045 mole) of S-methyl-N-hydroxythioacetimidate, 0.11 g dicyclohexyl-18-crown-6, and benzene (200 mol) were combined and stirred 0.5 hr. at room temperature. Then 9.4 g (0.045 mole) of N-methyl-N-(diisopropylaminosulfenyl)carbamoyl fluoride were added. The mixure was stirred at room temperature for 1 hr., and then was water washed four times, dried (MgSO4), and the benzene solvent was removed under vacuum. The residue was recrystallized from diisopropyl ether to give 9 g (67.3 percent yield) of S-methyl N-[N'-methyl-N'-(diisopropylaminosulfenyl)carbamoyloxy]thioacetimidate, m.p. 79°-80° C.

1. customat room temperature
2. stirringThe mixure was stirred at room temperature for 1 hr
3. washwashed four times
4. dry with materialdried (MgSO4)
5. customthe benzene solvent was removed under vacuum
6. customThe residue was recrystallized from diisopropyl ether