HRID1026351
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 2-(2-bromo-4-hydroxyphenyl)acetic acid (0.67 g), HATU (1.33 g), triethylamine (0.35 g) and N,O-dimethylhydroxylamine hydrochloride (0.34 g) in dichloromethane (30 mL) was stirred overnight, to which water (30 mL) was added. The organic layer was separated. The water layer was extracted by ethyl acetate (20 mL×3). The combined organic layer was dried over anhydrous sodium sulfate, filtered and evaporated to dryness. The residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate) to afford the title compound (773 mg).
WORKUP
后处理
- additionwas added
- customThe organic layer was separated
- extractionThe water layer was extracted by ethyl acetate (20 mL×3)
- dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
- filtrationfiltered
- customevaporated to dryness
- customThe residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate)