Triphenylphosphine → HCID 19852596、化合物

反応式

[F:1][C:2]([F:29])([F:28])[O:3][C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11]([N:13]2[CH2:17][C:16]([CH:19]=O)([CH3:18])[C:15]([C:21]3[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][CH:22]=3)=[N:14]2)=[O:12])=[CH:6][CH:5]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.Cl[C:50]([F:55])([F:54])C([O-])=O.[Na+]>COCCOCCOC>[F:29][C:2]([F:1])([F:28])[O:3][C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11]([N:13]2[CH2:17][C:16]([CH:19]=[C:50]([F:55])[F:54])([CH3:18])[C:15]([C:21]3[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][CH:22]=3)=[N:14]2)=[O:12])=[CH:6][CH:5]=1

参加物

実験手順

To 2.0 g of N-(4-trifluoromethoxyphenyl)-3-(4-chlorophenyl)-4-formyl-4-methyl-4,5-dihydro-1H-pyrazole-1-carboxamide (5 mmole), was added 4 g of triphenylphosphine (15 mmole), 3 g of sodium chlorodifluoroacetate (20 mmole) and 15 ml of diglyme. The mixture was heated slowly to reflux over 1 hour. Gas evolved. After refluxing for 20 minutes the mixture was colled, partitioned between ether and water, dried, rotovaped and chromatographed (ether/hexane) to yield 0.5 g of N-(4-trifluoromethoxyphenyl)-3-(4-chlorophenyl)-4-(2,2-difluorovinyl)-4-methyl-4,5-dihydro-1H-pyrazole-1-carboxamide mp 142°-8° C. NMR data was consistent with the structure.