反应详情

A solution of N-(2-amino-4-(tert-butyl)phenyl)-3-(3-((((3aR,4R,6R,6aS)-6-(4-((2,4-dimethoxybenzyl)amino)-7H-pyrrolo[2,3-d]pyrimidin-7-yl)-2,2-dimethyltetrahydro-3aH-cyclopenta[d][1,3]dioxol-4-yl)methyl)(methyl)amino)cyclobutyl)propanamide (0.24 g, 0.32 mmol) in Acetic acid (5 ml, 90 mmol) was stirred overnight at 60° C. The volatiles were removed in vacuo and remaining residue partitioned between Na2CO3 (2N) and DCM. The aqueous layer was extracted 3× with DCM and the combined organics dried with MgSO4, filtered and concentrated. The residue was purified by flash chromatography (DCM/7N NH3 in MeOH 94:6) to yield the desired compound (0.20 g) as a solid.

1. customThe volatiles were removed in vacuo
2. custompartitioned between Na2CO3 (2N) and DCM
3. extractionThe aqueous layer was extracted 3× with DCM
4. dry with materialthe combined organics dried with MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by flash chromatography (DCM/7N NH3 in MeOH 94:6)