反应详情

To a solution of tert-butyl N-[1-[3-[[2-amino-6-(cyanomethyl)pyrazolo[1,5-a]pyrimidine-3-carbonyl]amino]-4-pyridyl]-4-piperidyl]carbamate prepared according to a method similar to the one described in Example 1 (70 mg, 0.1424 mmol) in DCM (4 mL) was added TFA (1 mL, 12.98 mmol) and the mixture was stirred at ambient temperature for 1.5 hours. The reaction mixture was evaporated to dryness and purified by HPLC: 10-90% ACN in Water (TFA modifier) and the fractions were freeze-dried. The solid residue was dissolved in methanol (1 mL) and loaded onto a pre-wetted (15 mL methanol) 2 g SCX-2 cartridge. The cartridge was washed with methanol (2×15 mL) then the product eluted as a free base using 2M ammonia in methanol solution (3×15 mL). The product-containing fractions were evaporated to dryness, re-dissolved in water/methanol and freeze-dried to afford the desired product as a yellow solid (17 mg, 31%). MS (ES+) 391.1.

1. customThe reaction mixture was evaporated to dryness
2. custompurified by HPLC
3. dry with material10-90% ACN in Water (TFA modifier) and the fractions were freeze-dried
4. dissolutionThe solid residue was dissolved in methanol (1 mL)
5. washThe cartridge was washed with methanol (2×15 mL)
6. washthe product eluted as a free base
7. customThe product-containing fractions were evaporated to dryness
8. dissolutionre-dissolved in water/methanol
9. customfreeze-dried