反应详情

温度

60 °C

A solution of sodium hydroxide (0.32 g, 7.13 mmol) in water (5 mL) was added to a solution of Example 1 (1 g, 2.71 mmol) in methanol (30 mL). The reaction mixture was stirred at 60° C. for 1.5 h, the solvent was removed under vacuum and water (20 mL) was added. The reaction mixture was acidified to pH 3 using 10% aqueous hydrochloric acid. The precipitate was filtered and washed with water, dried to obtain the title compound. Yield: 0.85 g, (89%); 1H NMR (DMSO-d6, 300 MHz): δ 2.61 (s, 3H, CH3), 5.66 (s, 2H, CH2), 6.64 (d, 2H, Ar), 8.03 (s, 1H, Ar), 8.12 (s, 1H, Ar); MS: m/e (ES−) 352 (M−1).

1. customthe solvent was removed under vacuum and water (20 mL)
2. additionwas added
3. filtrationThe precipitate was filtered
4. washwashed with water
5. customdried