反应详情

The compound from Step 1 (9 g) was treated with trifluoroacetic acid (30 mL) and water (30 mL). The trifluoacetic acid was removed in vacuo and the reaction mixture partitioned between ethyl acetate and saturated sodium bicarbonate. The organic layer was washed with saturated sodium bicarbonate (×2), brine and dried over MgSO4. The solvent was removed in vacuo to give a yellow oil which was crystallised from ethyl acetate/hexanes to give the title compound. 4.6 g 1H NMR (360, CDCl3) δ 9.97 (s, 1H), 7.38 (m, 2H), 7.20 (m, 2H), 6.80 (s, 1H), 3.95 (s, 3H).

1. customThe trifluoacetic acid was removed in vacuo
2. customthe reaction mixture partitioned between ethyl acetate and saturated sodium bicarbonate
3. washThe organic layer was washed with saturated sodium bicarbonate (×2), brine
4. dry with materialdried over MgSO4
5. customThe solvent was removed in vacuo
6. customto give a yellow oil which
7. customwas crystallised from ethyl acetate/hexanes