反应详情

To a stirred mixture of compound (8) (100 mg, 0.25 mmol) and potassium carbonate (42 mg, 0.30 mmol) in DMF (2.5 mL) was added a solution of compound (3) (94 mg, 0.28 mmol) in DMF (2.5 mL) and the reaction mixture was stirred at RT for 18 hr. Potassium carbonate (3×35 mg, 0.75 mmol) was added in three portions over 30 hr. The solvent was removed in vacuo and the crude material was purified by flash column chromatography, eluting with 4.5% methanol in DCM, to afford the title compound (Intermediate B) (94 mg, 64%) as a off-white solid: m/z 588/590 (M+H)+ (ES+) (Method B).

1. customThe solvent was removed in vacuo
2. customthe crude material was purified by flash column chromatography
3. washeluting with 4.5% methanol in DCM