HRID1173837
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
Heat a mixture of 4-[2-(1-cyclohexyl-2-oxo-pyrrolidin-3-ylmethyl)-benzo[b]thiophen-5-yl]-benzoic acid methyl ester (250 mg, 0.64 mmol), LiOH.H2O (10 eq) into a dioxane (5 mL) and water (2 mL) at 80° C. for 1 hour. Add 2 M HCl (1 mL) and extract the mixture with ethyl acetate. Dry over sodium sulfate, filter, and concentrate. Purify by silica gel (20-50% ethyl acetate in hexanes) to give the title compound as a white powder (110 mg, 65%): MS (APCI-pos mode) m/z (rel intensity): 434.1 (M+H, 100%).
WORKUP
后处理
- temperatureHeat
- extractionextract the mixture with ethyl acetate
- dry with materialDry over sodium sulfate
- filtrationfilter
- concentrationconcentrate
- customPurify by silica gel (20-50% ethyl acetate in hexanes)