反应详情

A mixture of 3-[3-[1-pyrrolidinylmethyl]phenoxy]propanamine (0.97 g) and N-cyano-1-methyl-2-(phenylmethylene)hydrazine carboximidothioic acid methyl ester (0.97 g) was heated at 70° for 8 hr under a reduced pressure of 20 mm of mercury. Acetone was added and the solution was treated with hydrochloric acid at room temperature for one hour, washed with ether, basified with sodium carbonate and extracted with ethyl acetate. Evaporation of the ethyl acetate extracts gave a thick oil which crystallised from ethyl acetate/light petroleum (b.p. 60-80") to give the title compound as a white solid (0.2 g). TLC; silica/methanol/0.88 ammonia 80:1) Rf 0.5, m.p. 95°-95.5°.

1. temperaturewas heated at 70° for 8 hr under a reduced pressure of 20 mm of mercury
2. washwashed with ether
3. extractionextracted with ethyl acetate
4. customEvaporation of the ethyl acetate
5. customextracts gave a thick oil which
6. customcrystallised from ethyl acetate/light petroleum (b.p. 60-80")