ClCCl.[C:4]([C:7]1[CH:8]=[CH:9][C:10]([Cl:18])=[C:11]([CH2:13][NH:14]C(=O)C)[CH:12]=1)(=[O:6])[CH3:5].S(=O)(=O)(O)O.[OH-].[Na+]>C1(C)C=CC=CC=1.O>[NH2:14][CH2:13][C:11]1[CH:12]=[C:7]([C:4](=[O:6])[CH3:5])[CH:8]=[CH:9][C:10]=1[Cl:18]
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.
読み込み中…
