反应详情

To a suspension of tert-butyl 6-(4-nitrophenoxy)pyrimidin-4-ylcarbamate (1.22 g, 85% purity, 3.12 mmol) in DCM (12.0 mL) was added TFA (1.4 mL, 18.4 mmol) and the reaction mixture stirred at RT for 1 hr. An additional aliquot of TFA (0.70 mL) was added and the mixture was kept at RT for 15 hr and was then evaporated in vacuo. The residue was partitioned between EtOAc (50 mL) and saturated aq NaHCO3 solution (50 mL) and the organic layer was separated and washed with brine (25 mL) and then dried (MgSO4). Evaporation of the volatiles in vacuo the title compound as a yellow solid (0.66 g, 89%); Rt 1.38 min (Method 2); m/z 233 (M−H)+ (ES+).

1. waitthe mixture was kept at RT for 15 hr
2. customwas then evaporated in vacuo
3. customThe residue was partitioned between EtOAc (50 mL) and saturated aq NaHCO3 solution (50 mL)
4. customthe organic layer was separated
5. washwashed with brine (25 mL)
6. dry with materialdried (MgSO4)
7. customEvaporation of the volatiles in vacuo the title compound as a yellow solid (0.66 g, 89%)