反应详情

温度

100 °C

Potassiumhydroxide (1.96 g, 34.9 mmol) was dissolved in 30 ml of a 1:1 mixture of argon-flushed dioxane and water. After addition of 3-(4-bromo-benzyl)-2-ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidine (3) (4 g, 11.62 mmol), Pd2(dba)3 (426 mg, 0.465 mmol) and tetramethyl Xphos (894 mg, 1.859 mmol), the mixture was flushed with argon and stirred for 1 h at 100° C. Then the mixture was treated with 1N HCl and extracted with ethyl acetate. The combined organic layers were washed with brine, dried over Na2 SO4 and evaporated. Purification by chromatography (silica gel, ethylaceta/n-heptane) gave a yellow solid.

1. customflushed dioxane and water
2. customthe mixture was flushed with argon
3. additionThen the mixture was treated with 1N HCl
4. extractionextracted with ethyl acetate
5. washThe combined organic layers were washed with brine
6. customdried over Na2 SO4
7. customevaporated
8. customPurification by chromatography (silica gel, ethylaceta/n-heptane)
9. customgave a yellow solid