HRID1525228
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
A solution of compound 7-f (100 mg, 0.33 mmol) in methanol (2 mL) and water (2 mL) was treated with LiOH—H2O (14 mg, 0.33 mmol), and the resulting reaction solution was stirred at room temperature overnight. The resulting mixture was concentrated and extracted by EA. The aqueous layers was added HCl (1 M) until pH 1˜2. The mixture was extracted by EA. Combined organic layers was washed by brine, dried over Na2SO4 and concentrated to afford the title compound, 7-g, as oil (35 mg, 37%). 1H NMR (300 MHz, CDCl3) δ1.30-1.34 (m, 6H), 1.52 (d, J=7.2 Hz, 3H), 3.79 (q, J=7.2 Hz, 1H), 4.07-4.17 (m, 4H), 7.39-7.43 (m, 2H), 7.71-7.78 (m, 2H).
WORKUP
后处理
- customthe resulting reaction solution
- concentrationThe resulting mixture was concentrated
- extractionextracted by EA
- additionThe aqueous layers was added HCl (1 M) until pH 1˜2
- extractionThe mixture was extracted by EA
- washCombined organic layers was washed by brine
- dry with materialdried over Na2SO4
- concentrationconcentrated