反应详情

Aqueous sodium hydroxide (0.78 g, 19.6 mmol in 45 mL water) was added to a solution of Example 102 (3.21 g, 6.53 mmol) in tetrahydrofuran (45 mL). It was stirred for 3 h, partially concentrated, treated with dil. HCl to pH 7, filtered, washed with water and dried to obtain the title compound as a white solid. Yield: 3.01 g (97%). 1H NMR (CDCl3+DMSO-d6): δ 2.40 (s, 3H, CH3), 3.4 (t, 4H, 2CH2), 3.5 (t, 4H, 2CH2), 4.5 (s, 2H, CH2), 6.4 (d, 1H, Ar), 6.5 (d, 1H, Ar), 7.7 (d, 1H, Ar), 8.1 (d, 1H, Ar); MS: m/e (CI+) 478 (M+).

1. concentrationpartially concentrated
2. additiontreated with dil. HCl to pH 7
3. filtrationfiltered
4. washwashed with water
5. customdried