Acetic Acid → HCID 20070367、化合物

反応式

[CH3:1][C:2]([NH:6][C:7]1[CH:13]=[CH:12][CH:11]=[CH:10][C:8]=1[NH2:9])([CH3:5])[CH2:3][OH:4].Cl.N.[C:16](O)(=O)[CH3:17]>>[CH3:16][C:17]1[N:6]([C:2]([CH3:1])([CH3:5])[CH2:3][OH:4])[C:7]2[CH:13]=[CH:12][CH:11]=[CH:10][C:8]=2[N:9]=1

参加物

反応物 4

HCID 176Acetic Acid

HCID 222Ammonia

HCID 313Hydrochloric Acid

HCID 119615571-Propanol, 2-[(2-aminophenyl)amino]-2-methyl-

生成物 1

HCID 20070367HCID 20070367、化合物

実験手順

A mixture of 2-(1,1-dimethyl-2-hydroxyethyl)aminoaniline (from Preparation 2(a)) (8.4 g), acetic acid [4.2 g], and 4N hydrochloric acid [50 ml] were refluxed for 30 hours. The reaction was cooled and neutralised with concentrated aqueous ammonia. The solution was extracted with a mixture of tetrahydrofuran (1 part) and dichloromethane (3 parts) (3×100 ml). The organic phases were combined, dried over magnesium sulphate and the solvent removed under reduced pressure. The crude product was recrystallised from ethyl acetate yielding the title compound as a white solid 3.8 g (40%), m.p. 180°-181° C.