Tributylphosphine → HCID 13711424、化合物

反応式

[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C:9]1[S:13]S[C:11](=[O:14])[N:10]=1.[Cl:15][C:16]1[C:22]([C:23]([F:26])([F:25])[F:24])=[CH:21][C:20]([Cl:27])=[CH:19][C:17]=1[NH2:18].C(P(CCCC)CCCC)CCC>ClCCl>[Cl:15][C:16]1[C:22]([C:23]([F:25])([F:26])[F:24])=[CH:21][C:20]([Cl:27])=[CH:19][C:17]=1[NH:18][C:11]([NH:10][C:9](=[S:13])[C:3]1[C:2]([F:1])=[CH:7][CH:6]=[CH:5][C:4]=1[F:8])=[O:14]

参加物

実験手順

To a solution of 5-(2,6-difluorophenyl)-1,2,4-dithiazole-3-one (0.9 g) in 20 ml of dichloromethane was added dropwise a solution of 2,5-dichloro-3-trifluoromethylaniline (0.9 g) and tributylphosphine (0.8 g) in 10 ml of dichloromethane under ice-cooling and the solution was stirred for 30 minutes at room temperature. The dichloromethane was then distilled off under reduced pressure and to the residue was added ligroin. The precipitated crystal was filtered and the crystal was washed with ligroin to obtain the desired product 1.3 g. (d.p. 176°-177° C.)