反应详情

A mixture comprising 460 mg of 4-picolylamine, 430 mg of triethylamine and 1 ml of acetonitrile was dropwise added to 950 mg of 7-chloro-5-methylthiopyrazolo[1,5-a]pyrimidine-6-carbonitrile and 20 ml of acetonitrile under cooling with ice, followed by stirring for about 1 hour. After completion of the reaction, about 80 ml of water was added thereto, and the precipitated crystals were collected by filtration, washed with water and dried to obtain crude crystals. The crude crystals were purified by silica gel column chromatography to obtain 970 mg of 7-(4-pyridylmethyl)amino-5-methylthiopyrazolo[1,5-a]pyrimidine-6-carbonitrile (compound No. 3) having a melting point of from 153 to 154° C.

1. temperatureunder cooling with ice
2. additionwas added
3. filtrationthe precipitated crystals were collected by filtration
4. washwashed with water
5. customdried
6. customto obtain crude crystals
7. customThe crude crystals were purified by silica gel column chromatography