反应详情

温度

100 °C

A mixture of N-(3-chloropropyl)-2-benzoxazolinone (8.5 g, 40 mmol), polyphosphoric acid (100 g), and acetic acid (2.4 g, 2.3 ml, 40 mmol), was stirred and heated at 100° C. for 2 hours. The hot solution was poured into ice-water to deposit a yellow gum. The mixture was extracted with dichloromethane, and insolubles were filtered. The dichloromethane extract was washed with water, dried (K2CO3), and concentrated to afford 6.4 g of a slightly green solid. This was recrystallized from ethanol (95%) to yield N-(3-chloropropyl)-6-acetyl-2-benzoxazolinone as a brown solid, 3.5 g, m.p.=100°-103° C.

1. extractionThe mixture was extracted with dichloromethane, and insolubles
2. filtrationwere filtered
3. extractionThe dichloromethane extract
4. washwas washed with water
5. dry with materialdried (K2CO3)
6. concentrationconcentrated
7. customto afford 6.4 g of a slightly green solid
8. customThis was recrystallized from ethanol (95%)