反应详情

温度

85 °C

Acetate 10 (20 mg, 0.072 mmoles) was dissolved in 2 N HCl (0.31 mL) and heated to 85° C. After 3 h, the reaction mixture was diluted with 5 N NaOH to a pH˜11 and extracted with CH2Cl2 (3×3 mL). The combined organic layers were dried over Na2SO4 and concentrated to afford 11(16.2 mg, 0.071 mmoles, 96%) as a colorless oil. 1H NMR (CDCl3) δ 7.83 (1H, dd, J=1.7, 7.6 Hz), 7.32 (1H, ddd, J=2.2, 8.1, 9.1 Hz), 6.93 (1H, m), 6.77 (1H, d, J=7.9 Hz), 3.76 (1H, d, J=7.9 Hz), 3.98 (1H, s), 2.83 (6H, m), 1.31 (2H, m), 1.64 (5H, m); IR (thin film, NaCl) 3290, 2964, 1716, 1664, 1422 cm−1; LRMS: M+=230.

1. extractionextracted with CH2Cl2 (3×3 mL)
2. dry with materialThe combined organic layers were dried over Na2SO4
3. concentrationconcentrated