反应详情

温度

50 °C

To 199.8 kg of a dichloromethane solution of N-[(5-acetyl-2-chlorophenyl)methyl]acetamide obtained in Example 3-(B), 90 kg of water and 46 kg (0.45 kmoles) of 98% sulfuric acid were added. Dichloromethane was distilled off under normal pressure over 1.5 hours until the inner temperature reaches 100° C., followed by aging for 6 hours. After the completion of the reaction, the reaction solution was cooled to 50° C. over 20 minutes and 90 kg of water and 105 kg of toluene were added. After cooling, 212 kg of an aqueous 25% sodium hydroxide solution was added dropwise at 15 to 25° C. over 2.5 hours. After heating to 40° C. over 30 minutes, the organic layer was partitioned to obtain a toluene solution of 1-[3-(aminomethyl)-4-chlorophenyl]ethan-1-one.

1. distillationDichloromethane was distilled off under normal pressure over 1.5 hours until the inner temperature
2. customreaches 100° C.
3. customAfter the completion of the reaction
4. temperatureAfter cooling
5. temperatureAfter heating to 40° C. over 30 minutes
6. customthe organic layer was partitioned