反应详情

Conversion of the hydrochloride salt of 2-imino-1-methylpyrrolidine (6.73 g.; 0.05 mole) to the free base (4.9 g. assuming 100% conversion) is carried out in the usual manner. After drying over K2CO3 the benzene layer is stirred at room temperature and 9.36 g. (0.05 mole) of m-trifluoromethylphenylisocyanate is added (some solid precipitates). The reaction mixture is stirred overnight. The resulting solid is collected, m.p. = 155°-156° C. The benzene filtrate, upon removal of the solvent, affords an additional crop of solid material, m.p. 131°-137° C. Recrystallizations of the combined solids from acetone-pet. ether gives the pure product, 1-(1-methyl-2-pyrrolidylidene)-3-(m-trifluoromethylphenyl)urea, m.p. = 155°-156.5° C.

1. dry with materialAfter drying over K2CO3 the benzene layer
2. customprecipitates)
3. stirringThe reaction mixture is stirred overnight
4. customThe resulting solid is collected
5. customThe benzene filtrate, upon removal of the solvent
6. customaffords an additional crop of solid material, m.p. 131°-137° C
7. customRecrystallizations of the combined solids from acetone-pet. ether