反应详情

温度

80 °C

A suspension of 5-amino-pyrazolo[1,5-a]pyrimidine-3-carboxylic acid [5-(5-chloro-2-difluoromethoxy-phenyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrazol-4-yl]-amide (720 mg, 1.31 mmol) in methanol (20 mL) was treated with concentrated aqueous HCl (3 mL) and the mixture heated at 80° C. for 1 hour. The solvent was evaporated and the residue azeotroped with methanol (×3). The resultant solid was triturated with ethyl acetate, collected by filtration, washed with ethyl acetate and diethyl ether and left to air dry. The residual solid was purified by flash chromatography on silica eluting with 0-12% 2M NH3/MeOH in DCM. Collecting appropriate fractions, followed by evaporation gave 5-amino-pyrazolo[1,5-a]pyrimidine-3-carboxylic acid [3-(5-chloro-2-difluoromethoxy-phenyl)-1H-pyrazol-4-yl]-amide as a brown solid (378 mg, 69%). LCMS (Method 4) [M+H]+=419.9, RT=2.93

1. customThe solvent was evaporated
2. customthe residue azeotroped with methanol (×3)
3. customThe resultant solid was triturated with ethyl acetate
4. filtrationcollected by filtration
5. washwashed with ethyl acetate and diethyl ether
6. waitleft to air
7. customdry
8. customThe residual solid was purified by flash chromatography on silica eluting with 0-12% 2M NH3/MeOH in DCM
9. customCollecting appropriate fractions
10. customfollowed by evaporation