反应详情

To a stirred solution of 352 (53 mg, 0.15 mmol) in DCM (750 μL) at RT under nitrogen was added TFA (750 μL). The solution was stirred for 2 h and was then concentrated in a rotovap under high vacuum. The residue was redissolved in DCM (10 mL) and stirred rapidly with 1M Na2CO3 (10 mL) for 5 min. The layers were separated and the aqueous phase was extracted with DCM (2×10 mL). The combined extracts were dried (MgSO4), filtered and concentrated to afford 29 mg (76%) of 3,3,3-trifluoro-2-(5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-2-ylamino)propan-1-ol (354) as a yellow foam.

1. concentrationwas then concentrated in a rotovap under high vacuum
2. dissolutionThe residue was redissolved in DCM (10 mL)
3. stirringstirred rapidly with 1M Na2CO3 (10 mL) for 5 min
4. customThe layers were separated
5. extractionthe aqueous phase was extracted with DCM (2×10 mL)
6. dry with materialThe combined extracts were dried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated