Ammonium Chloride → 5-(5-Isopropyl-2,4-bis-methoxymethoxy-phenyl)-4-(4-methoxy-phenyl)-2,4-dihydro-[1,2,4]triazol-3-thione
反応式
COC1C=CC([N:9]([C:14](=O)[C:15]2[CH:20]=[C:19]([CH:21]([CH3:23])[CH3:22])[C:18]([O:24][CH2:25][O:26][CH3:27])=[CH:17][C:16]=2[O:28][CH2:29][O:30][CH3:31])[NH:10][C:11]([NH2:13])=[S:12])=CC=1.[Cl-].[NH4+]>[OH-].[Na+]>[CH:21]([C:19]1[C:18]([O:24][CH2:25][O:26][CH3:27])=[CH:17][C:16]([O:28][CH2:29][O:30][CH3:31])=[C:15]([C:14]2[N:13]([C:15]3[CH:20]=[CH:19][C:18]([O:24][CH3:25])=[CH:17][CH:16]=3)[C:11](=[S:12])[NH:10][N:9]=2)[CH:20]=1)([CH3:23])[CH3:22]参加物
4
実験手順
4-methoxyphenyl-1-[5-isopropyl-2,4-bis(methoxymethoxy)-benzoyl]thiosemicarbazide (F53-03: 24.9 g, 53.7 mmol) and 5% aqueous sodium hydroxide (500 mL) were placed in a 1 L eggplant shaped flask and heated under reflux for 1 hour. After completing the reaction, the reaction mixture was neutralized with saturated aqueous ammonium chloride, and the solids deposited were collected by filtration, washed with distilled water and then dried under reduced pressure. The crude product thus obtained was purified by suspending in ethyl acetate/hexane and concentrating under reduced pressure to obtain the title compound (F53-04:20.5 g, 85.4%).