反应详情

The reaction was run in a 500 mL 3 neck round bottom (RB) fitted with a mechanical stirrer and reflux condenser. To 45 g (301.6 mmol) of 3-methylacetanilide in 240 mL of carbon disulfide under argon at RT was added 38.6 mL (542.8 mmol) of acetyl chloride with stirring. To the solution was then added 145 g (1.09 mol) of aluminum chloride in small portions over a 1 h period. After addition was complete the mixture was refluxed for 1 h and then allowed to cool and stand for 1 h. The supernatant carbon disulfide layer was decanted off and the very dark viscous lower layer was poured into a mixture of cracked ice and hydrochloric acid. The precipitate was collected and washed with 1 L of water. The solid was dried under high vacuum for 30 h at RT no provide 52.17 g (90%) of title amide in the form of a light tan solid which is used as the crude material in the following reaction.

1. customfitted with a mechanical stirrer
2. temperaturereflux condenser
3. additionAfter addition
4. temperaturewas refluxed for 1 h
5. temperatureto cool
6. customThe supernatant carbon disulfide layer was decanted off
7. additionthe very dark viscous lower layer was poured into a mixture of cracked ice and hydrochloric acid
8. customThe precipitate was collected
9. washwashed with 1 L of water
10. dry with materialThe solid was dried under high vacuum for 30 h at RT no provide 52.17 g (90%) of title amide in the form of a light tan solid which
11. customis used as the crude material in the following reaction