반응 #52995

반응 방정식

4-amino-2-chlorobenzoic acid methyl ester

2,5-dimethoxytetrahydrofuran

→

2-chloro-4-(1-pyrrolyl)benzoic acid methyl ester

용매

water

AcOH

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도under reflux for 2 h
3. 3
   추출extracted with EtOAc
4. 4
   세척The extract was washed with satd
5. 5
   건조NaHCO3 and brine, dried (MgSO4)
6. 6
   여과filtered
7. 7
   기타evaporated
8. 8
   기타The residue was purified by column chromatography (silica gel; eluent: hexane/EtOAc 5/1)

실험 절차

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+).

출처