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 3-(2-Hydroxycarbamoyl-1-(4-methoxy-benzenesulfonyl)-azepan-3-yl)-acrylic acid ethyl ester (41 mg, 0.096 mmoL) in 0.96 mL THF and 1.1 mL water was added lithium hydroxide (12 mg, 0.288 mmoL) at ambient temperature. After 3.5 hours the reaction solvent was evaporated under reduced pressure, and the residue was diluted with water and washed twice with diethyl ether. The water layer was acidified to pH=1 and extracted twice with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate, filtered, and the solvent evaporated under reduced pressure. The residue was freeze dried to yield 3-(2-Hydroxycarbamoyl-1-(4-methoxy-benzenesulfonyl)-azepan-3-yl)-acrylic acid; MS: (M+H)+ =399, (M+NH4)+ =416, (M-H)- =397.
WORKUP
后处理
- customAfter 3.5 hours the reaction solvent was evaporated under reduced pressure
- additionthe residue was diluted with water
- washwashed twice with diethyl ether
- extractionextracted twice with ethyl acetate
- washThe organic layer was washed with brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- customthe solvent evaporated under reduced pressure
- customdried