反应详情

To a solution of pyrazolo[1,5-a]pyrimidine-3-carboxylic acid (56.8 mg, 0.348 mmol) in DCM (2.0 ml) was added HATU (132 mg, 0.348 mmol) and DIPEA (0.152 ml, 0.870 mmol) and the mixture stirred for 15 minutes before addition of (2R)-2-methyl-1-{[4-(trifluoromethyl)phenyl]sulfonyl}piperazine hydrochloride (may be prepared as described in Description 4) (100 mg, 0.290 mmol) in DMF (2 ml). The resultant mixture was stirred for 72 hours at rt. Water (20 ml) and EtOAc (20 ml) were added and the mixture was filtered through a sinter to remove precipitate. The collected filtrate was separated and the aqueous layer was then re-extracted with EtOAc (15 ml), the organic layers were combined and washed with saturated brine solution (20 ml). The organic layers were then separated, dried (MgSO4) and concentrated to dryness. The crude material was then dissolved in DMSO and purified by MDAP. The collected fractions were concentrated in vacuo to give the title compound (85.8 mg) as a white solid.

1. filtrationthe mixture was filtered through a sinter
2. customto remove precipitate
3. customThe collected filtrate was separated
4. extractionthe aqueous layer was then re-extracted with EtOAc (15 ml)
5. washwashed with saturated brine solution (20 ml)
6. customThe organic layers were then separated
7. dry with materialdried (MgSO4)
8. concentrationconcentrated to dryness
9. dissolutionThe crude material was then dissolved in DMSO
10. custompurified by MDAP
11. concentrationThe collected fractions were concentrated in vacuo