Water → HCID 178426271、化合物

反応式

P(Cl)(Cl)(Cl)=O.[CH3:6][C:7]1[CH:8]=[C:9]([N:14]2[C:18](=[O:19])[CH:17]=[C:16]([CH3:20])[NH:15]2)[CH:10]=[CH:11][C:12]=1[CH3:13].O.CN(C)[CH:24]=[O:25]>>[CH3:6][C:7]1[CH:8]=[C:9]([N:14]2[C:18]([OH:19])=[C:17]([CH:24]=[O:25])[C:16]([CH3:20])=[N:15]2)[CH:10]=[CH:11][C:12]=1[CH3:13]

参加物

反応物 4

HCID 962Water

HCID 6228Dimethylformamide

HCID 24813Phosphorus oxychloride

HCID 117358291-(3,4-Dimethylphenyl)-3-methyl-3-pyrazolin-5-one

生成物 1

HCID 178426271HCID 178426271、化合物収率 79%

反応条件

温度: 100 °C

実験手順

Phosphorus oxychloride (4.82 mL, 51.6 mmol) was added dropwise to an ice-cooled, stirred suspension of 1-(3,4-dimethylphenyl)-3-methyl-3-pyrazolin-5-one (8.70 g, 43.0 mmol) in dimethylformamide (18.0 mL) at such a rate as to maintain the temperature below 20° C. After the addition, the mixture was heated at 100° C. for 2 h, then cooled, poured into iced water (200 mL). The resulting mixture was stirred for 18 h, then filtered. The solid was washed with water and dried to give the title compound (7.83 g, 79%) as a cream-coloured powder. MS (ES) m/e 231 [M+H]+.