反应详情

A mixture of 3-acetamidoacetophenone (3 kg; Lancaster), dimethylformamide dimethylacetal (7 L; Lancaster) and toluene (12 L; Mallinckrodt) is heated at reflux and methanol collected as it is formed. The mixture is heated overnight and a precipitate forms during this time. The reaction may be monitored by TLC analysis (EtOAc: starting material Rf=0.46; product Rf=0.10) to ensure it goes to completion. The reaction mixture is cooled and the solid is collected by filtration. The cake is washed with hexanes (4 L) then dried to give 3.77 kg (95% yield) of a light yellow powder.

1. temperatureis heated
2. temperatureat reflux
3. custommethanol collected as it
4. customis formed
5. temperatureThe mixture is heated overnight
6. customThe reaction
7. temperatureThe reaction mixture is cooled
8. filtrationthe solid is collected by filtration
9. washThe cake is washed with hexanes (4 L)
10. customthen dried