Pyridine → HCID 15580737、化合物

反応式

[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[CH2:13][CH2:12][C:11]([NH:14][C:15](=[O:20])[C:16](F)(F)F)=[N:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].N1C=CC=CC=1.[Cl:27][C:28]1[CH:36]=[CH:35]C(C(Cl)=O)=[CH:30][CH:29]=1>O>[Cl:27][C:28]1[CH:36]=[CH:35][C:16]([C:15]([NH:14][C:11]2[CH2:12][CH2:13][N:9]([C:4]3[CH:5]=[CH:6][C:7]([Cl:8])=[C:2]([Cl:1])[CH:3]=3)[N:10]=2)=[O:20])=[CH:30][CH:29]=1

参加物

実験手順

A stirred mixture of 2.30 g. of 3-amino-1-(3,4-dichlorophenyl)-2-pyrazoline (prepared as described in Example 1) in 20 ml. of dry pyridine is cooled in an ice bath, then 2.10 g. of p-chlorobenzoyl chloride is added. The reaction mixture is allowed to stand at room temperature for 16 hours then is poured into water to separate a solid. The solid is collected by filtration and dissolved in dichloromethane. This solution is passed through a short column of a hydrous magnesium silicate. The effluent is refluxed and hexane is added until turbidity results. The solution is cooled and filtered to collect a product. The product is recrystallized from the same solvent pair to give 1.8 g. of the desired product as yellow needles, m.p. 177°-178° C.