Hydrazine hydrate (1:1) → 2,2-Bis[4-(3-aminophenoxy)phenyl]propane
反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:33]=[CH:34][CH:35]=1)[O:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]([C:17]2[CH:22]=[CH:21][C:20]([O:23][C:24]3[CH:29]=[CH:28][CH:27]=[C:26]([N+:30]([O-])=O)[CH:25]=3)=[CH:19][CH:18]=2)([CH3:16])[CH3:15])=[CH:10][CH:9]=1)([O-])=O.O.NN>COCCO>[NH2:30][C:26]1[CH:25]=[C:24]([CH:29]=[CH:28][CH:27]=1)[O:23][C:20]1[CH:19]=[CH:18][C:17]([C:14]([C:11]2[CH:12]=[CH:13][C:8]([O:7][C:6]3[CH:33]=[CH:34][CH:35]=[C:4]([NH2:1])[CH:5]=3)=[CH:9][CH:10]=2)([CH3:15])[CH3:16])=[CH:22][CH:21]=1参加物
4
実験手順
In the second step, a 500 ml glass reaction vessel was charged with 100 grams (0.21 mol) of 2,2-bis[4-(3-nitrophenoxy)phenyl]propane, 10 grams of active carbon, 1 gram of ferric chloride hexa-hydrate and 300 ml of ethyleneglycol monomethylether. The mixture was refluxed with stirring for 30 minutes, followed by dropping 42 grams (0.84 mol) of hydrazine hydrate at 70°-80° C. during 2 hours, and stirred for further 5 hours at 70°-80° C. The resultant reaction mixture was cooled, filtered to remove the catalyst and 150 ml of ethyleneglycol monomethylether was distilled off. To the residual matter, 270 grams of 20% aqueous hydrogen chloride solution and 30 grams of sodium chloride were added, and cooled to 20°-25° C. with stirring. The separated crystals were filtered, dissolved into 30% aqueous IPA solution and neutralized with aqueous ammonia to separate crystals. The crystals were filtered, washed with water, dried and recrystallized from a mixture of benezene and n-hexane. Colorless crystals of 2,2-bis[4-(3-aminophenoxy)phenyl]propane thus obtained were 69.2 grams (75% yield) and had a melting point of 106°-108° C. and their analytical results were as follows.