反应详情

温度

80 °C

200 mg of 4-chloro-3-(2-chloro-phenyl)-6-methyl-1H-pyrazolo[3,4-d]pyrimidine (from step 4 of Example 1) was dissolved in 5 ml of 7N ammonia in methanol, and the solution was stirred at 80° C. over night in a sealed tube. The resulting reaction mixture was concentrated under vacuum and then extracted in 60 ml ethylacetate. The solution was washed first with water and next with brine, dried and after removing the solvent in vacuo afforded 190 mg (90%)) of 3-(2-chloro-phenyl)-6-methylsulfanyl-1H-pyrazolo[3,4-d]pyrimidin-4ylamine as a light tan solid, MS: 292 (M+H). The crude 3-(2-chloro-phenyl)-6-methylsulfanyl-1H-pyrazolo[3,4-d]pyrimidin-4ylamine was used in the next step without further purification.

1. customThe resulting reaction mixture
2. concentrationwas concentrated under vacuum
3. extractionextracted in 60 ml ethylacetate
4. washThe solution was washed first with water and next with brine
5. customdried
6. customafter removing the solvent in vacuo