反应详情

To a solution of (R)-5-(2-(5-fluoro-2-methylpyridin-3-yl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidine-3-carboxylic acid (Preparation O, 50 mg, 0.15 mmol) in DCM (2 mL) was added HOBt (40 mg, 0.29 mmol) followed by EDCI (84 mg, 0.44 mmol). The solution was stirred at ambient temperature for 15 minutes, then treated with triethylamine (61 μL, 0.44 mmol) followed by cyclopropylamine (31 μL, 0.44 mmol). After stirring for 16 hours the mixture was partitioned between saturated NH4Cl solution (20 mL) and DCM (20 mL) and the aqueous layer was extracted with DCM (2×10 mL). The combined organic phases were washed with brine (10 mL), dried over Na2SO4, filtered and concentrated. The residue was purified by silica gel column chromatography, eluting with 2-4% MeOH/DCM, to afford the title product as white solid (44 mg, 79%). MS (apci) m/z=381.1 (M+H).

1. stirringAfter stirring for 16 hours the mixture
2. customwas partitioned between saturated NH4Cl solution (20 mL) and DCM (20 mL)
3. extractionthe aqueous layer was extracted with DCM (2×10 mL)
4. washThe combined organic phases were washed with brine (10 mL)
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was purified by silica gel column chromatography
9. washeluting with 2-4% MeOH/DCM