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
Methyl 2-{[2-(4-{2-[(2-chlorobenzyl)(ethyl)amino]-2-oxoethoxy}phenyl)ethyl]thio}-benzoate was dissolved in a mixture of THF (freshly distilled)/water (2/1, 3 ml), Lithium hydroxide (0.015 g, 0.629 mmol) was added. The reaction was performed in a single node microwave oven (5 min, 150 deg). THF was removed by evaporation. Water was added (10 ml) and the basic water phase was washed with diethyl ether (2×10 ml). Addition of HCl (2 ml, 1 M, pH 1). The water phase was extracted with two portions of DCM (20 ml). The organic phase was dried (MgSO4) and the solvent was removed by evaporation to give 0.103 g of 2-{[2-(4-{2-[(2-chlorobenzyl)(ethyl)amino]-2-oxoethoxy}phenyl)ethyl]thio}-benzoic acid (yield 95.5%).
WORKUP
后处理
- additionwas added
- customThe reaction was performed in a single node microwave oven
- custom(5 min, 150 deg)
- customTHF was removed by evaporation
- additionWater was added (10 ml)
- washthe basic water phase was washed with diethyl ether (2×10 ml)
- additionAddition of HCl (2 ml, 1 M, pH 1)
- extractionThe water phase was extracted with two portions of DCM (20 ml)
- dry with materialThe organic phase was dried (MgSO4)
- customthe solvent was removed by evaporation