反应详情

To a stirring solution of 6.73 g. (0.05 mole) of 1-methyl- 2-iminopyrrolidine hydrochloride in about 2 ml. of water is added about 50 ml. of benzene followed by 10 ml. of 50% NaOH. After stirring 1 min. the benzene layer is decanted onto anhydrous potassium carbonate. The extraction is repeated twice. The combined benzene extracts are filtered from a drying agent (dicalite pad) and rinsed well with dry benzene. To the filtrate is added in one portion with stirring 7.36 g. (0.05 mole) of 2,6-dimethylphenylisocyanate. The reaction mixture is stirred overnight. Solvent removal and recrystallization from ethyl acetate-ether gives the product, 1-(2,6 -dimethylphenyl)-3-(1-methyl-2-pyrrolidylidene)urea, as white crystals, m.p. = 119°-120° C.

1. customis decanted onto anhydrous potassium carbonate
2. extractionThe extraction
3. filtrationThe combined benzene extracts are filtered from a drying agent (dicalite pad)
4. washrinsed well with dry benzene
5. additionTo the filtrate is added in one portion
6. stirringThe reaction mixture is stirred overnight
7. customSolvent removal and recrystallization from ethyl acetate-ether