HRID1169884
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Compound 79 (200 mg, 0.63 mmol) was treated with a solution at 15% of TFA in CH2Cl2 at room temperature for 45 min. The solution was concentrated in vacuo and water (10 mL) was added. The aqueous phase was washed with Et2O, basified with aqueous 2N NaOH, and extracted with CHCl3 (10 mL×3) obtaining 130 mg of a white solid (80) (yield 96%). 1H NMR (CDCl3, 300 MHz) δ8.37 (br s, 1H), 7.29-7.22 (m, 2H), 6.82 (d, J=9.3 Hz, 1H), 5.44 (br s, 1H), 3.8(s, 2H), 3.89 (s, 2H). MS (m/e) (API-ES) 215 (M+H)+, m.p. 135-137° C.
WORKUP
后处理
- concentrationThe solution was concentrated in vacuo and water (10 mL)
- additionwas added
- washThe aqueous phase was washed with Et2O
- extractionextracted with CHCl3 (10 mL×3)