反应详情

A mixture comprising 2.15 g of 7-hydroxy-5-methylthiopyrazolo[1,5-a]pyrimidine-6-carbonitrile (compound No. 49), 1.3 g of N,N-dimethylaniline and 5 ml of phosphorus oxychloride was stirred under reflux with heating for about 3 hours. After the completion of the reaction, the reaction mixture was cooled to room temperature, and poured into ice water, followed by stirring. 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 2.17 g of 7-chloro-5-methylthiopyrazolo[1,5-a]pyrimidine-6-carbonitrile (compound No. 62) having a melting point of from 201 to 202° C.

1. temperatureunder reflux
2. temperaturewith heating for about 3 hours
3. customAfter the completion of the reaction
4. stirringby stirring
5. filtrationThe precipitated crystals were collected by filtration
6. washwashed with water
7. customdried
8. customto obtain crude crystals
9. customThe crude crystals were purified by silica gel column chromatography