HRID24717
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
A mixture of 4-amino-2-chlorobenzoic acid methyl ester (0.46 g) and 2,5-dimethoxytetrahydrofuran (0.33 mL) in AcOH (16 mL) was heated under reflux for 2 h. The mixture was cooled to room temperature, diluted with water and extracted with EtOAc. The extract was washed with satd. NaHCO3 and brine, dried (MgSO4), filtered and evaporated. The residue was purified by column chromatography (silica gel; eluent: hexane/EtOAc 5/1) to yield 0.48 g of 2-chloro-4-(1-pyrrolyl)benzoic acid methyl ester. ESMS: m/z 236 (MH+).
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 2 h
- extractionextracted with EtOAc
- washThe extract was washed with satd
- dry with materialNaHCO3 and brine, dried (MgSO4)
- filtrationfiltered
- customevaporated
- customThe residue was purified by column chromatography (silica gel; eluent: hexane/EtOAc 5/1)