反应详情

The hydrochoride salt of 2-imino-1-methylpyrrolidine (6.73 g.; 0.05 L mole) is converted to free base (4.0 g.; 0.05 mole) by adding 10 ml. of 50% NaOH to an aqueous slurry (minimal amount of water) of the salt and benzene extraction. After drying over K2CO3, the benzene solution is stirred at room temperature and 8.06 g. (0.05 mole) of 2,4,6-trimethylphenylisocyanate [made according to the method of K. Inukai and Y. Maki, Kogyo Kagaku Zasshi, 70 (4), 491-4 (1967)] dissolved in anhydrous benzene is added. The reaction mixture is stirred at room temperature for 11/2 hours and then the solvent is evaporated in vacuo leaving an oily residue, which crystallizes on cooling. Recrystallizaton from acetone yields the pure product, 1-mesityl-3-(1-methyl-2-pyrrolidylidene)urea, m.p. = 121°-123° C.

1. additionby adding 10 ml
2. extractionof 50% NaOH to an aqueous slurry (minimal amount of water) of the salt and benzene extraction
3. dry with materialAfter drying over K2CO3
4. additionis added
5. stirringThe reaction mixture is stirred at room temperature for 11/2 hours
6. customthe solvent is evaporated in vacuo
7. customleaving an oily residue, which
8. customcrystallizes
9. temperatureon cooling