反应详情

To a stirred solution of the 1-(3,4-dichlorophenyl)cyclopropane-1,2-dicarboxylic acid (28.3 g) in acetyl chloride (142 ml) was heated to reflux for 3 h, cooled to room temperature and evaporated. The oil was dissolved in toluene (100 ml) and evaporated to dryness. This was then repeated twice before triturating the semi-solid in hexane (100 ml). The solid was filtered off, washed with hexane and pulled dry under a nitrogen atmosphere to give a brown solid, yield=26.7 g (101%); 1HNMR (300 MHz, CDCl3) δ 7.52-7.46 (m, 2H, ArH), 7.27-7.24 (m, 1H, ArH), 3.35-3.30 (m, 1H, CH), 2.13-2.10 (m, 1H, CH), 1.97-1.95 (m, 1H, CH).

1. temperatureto reflux for 3 h
2. customevaporated
3. dissolutionThe oil was dissolved in toluene (100 ml)
4. customevaporated to dryness
5. custombefore triturating the semi-solid in hexane (100 ml)
6. filtrationThe solid was filtered off
7. washwashed with hexane
8. custompulled dry under a nitrogen atmosphere
9. customto give a brown solid, yield=26.7 g (101%)