反应详情

Compound 51 (20.0 g, 50.6 mmol) was dissolved in PhNO2 (130 mL) and the solution was cooled in an ice bath. Then AlCl3 (34.0 g, 254.7 mmol) and after that, 3-chloropropionyl chloride (25.0 mL, 259.8 mmol) were added. The mixture was kept for 40 min (LC/MS monitoring), poured in a mixture of diluted HCl and ice, extracted with CHCl3, and left for 16 h. The straw-colored precipitated obtained was filtered and washed with ether. Yield of 57: 18.47 g (63%).

1. temperaturethe solution was cooled in an ice bath
2. extractionextracted with CHCl3
3. waitleft for 16 h
4. customThe straw-colored precipitated
5. customobtained
6. filtrationwas filtered
7. washwashed with ether