反应详情

The hydrochloride salt of 2-imino-1-methylpiperidine (14.8 g.; 0.1 mole) is converted to free base by adding 10 ml. of 50% NaOH and extracting into benzene. After drying over K2CO3, the benzene layer is stirred at room temperature and 8.84 g. (0.05 mole) of N-methyl-phenylcarbamoyl chloride (prepared according to the method of J. A. Aeschlimann, U.S. Pat. No. 2,449,440), dissolved in anhydrous benzene, is added dropwise to this solution. The mixture is stirred at room temperature overnight (about 17 hours) and then filtered. The filtrate is taken to dryness in vacuo and the residue is dissolved in and recrystallized from hexane to give the product, 1-methyl-3-(1-methyl-2-piperidylidene)-1-phenylurea.

1. additionby adding 10 ml
2. extractionof 50% NaOH and extracting into benzene
3. dry with materialAfter drying over K2CO3
4. additionis added dropwise to this solution
5. stirringThe mixture is stirred at room temperature overnight (about 17 hours)
6. filtrationfiltered
7. dissolutionthe residue is dissolved in and
8. customrecrystallized from hexane