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
To a solution of Acetic acid 2-hydroxycarbamoyl-1-(4-methoxy-benzenesulfonyl)-azepan-3-ylmethyl ester in 1.1 mL methanol was added 0.1 mL of 1.0 M LiOH in water at ambient temperature. The reaction was stopped after 30 minutes by evaporating the solvent under reduced pressure. The residue was taken up in water and washed twice with diethyl ether, followed by acidification of the water to pH=1 with 1N HCl. The water layer was extracted twice with ethyl acetate which was dried over anhydrous magnesium sulfate and filtered. The solvent was evaporated under reduced pressure and was purified with column chromatography (silica: 2% to 8% methanol in dichloromethane) to yeild a thin film which was freeze-dried to yield 3-Hydroxymethyl-1-(4-methoxy-benzenesulfonyl)-azepane-2-carboxylic acid hydroxamide as a white lyopholate; MS: (M-H)- =357.
WORKUP
后处理
- customby evaporating the solvent under reduced pressure
- washwashed twice with diethyl ether
- extractionThe water layer was extracted twice with ethyl acetate which
- dry with materialwas dried over anhydrous magnesium sulfate
- filtrationfiltered
- customThe solvent was evaporated under reduced pressure
- customwas purified with column chromatography (silica: 2% to 8% methanol in dichloromethane) to yeild a thin film which
- customwas freeze-dried