反应详情

To a solution of the title compound of Example 1, Step H (4.14 g, 10 mmol) in anhydrous dichloromethane (200 mL) and pyridine (5 mL) was added a solution of acetyl chloride (0.863 g, 11 mmol) in dichloromethane (10 mL) dropwise at room temperature. After completion of the reaction (monitored by tlc), the organic phase was washed with water (50 mL) and diluted with HCl (5%, 50 mL). The organic layer was separated, dried (MgSO4), and the solvent was removed in vacuo to give the title compound of Step A, a compound of this invention, as a white solid (4.3 g, 94%) melting at 198-200° C. 1H NMR (CDCl3) δ 7.56 (m, 2H), 5.52 (m, 1H), 5.40 (dd, 1H), 4.84 (d, 1H), 4.62 (dd, 1H), 4.08 (m, 1H), 3.62 (m, 1H), 2.68 (m, 1H), 2.05 (s, 3H), 1.98 (m, 1H).

1. customAfter completion of the reaction (monitored by tlc)
2. washthe organic phase was washed with water (50 mL)
3. additiondiluted with HCl (5%, 50 mL)
4. customThe organic layer was separated
5. dry with materialdried (MgSO4)
6. customthe solvent was removed in vacuo