[Cl:1][C:2](Cl)(Cl)[S:3]Cl.[CH3:7][C:8]1[CH:16]=[C:15]([CH3:17])[CH:14]=[C:13]([CH3:18])[C:9]=1[C:10]([NH2:12])=[NH:11].[OH-].[Na+]>ClCCl.O>[Cl:1][C:2]1[S:3][N:12]=[C:10]([C:9]2[C:8]([CH3:7])=[CH:16][C:15]([CH3:17])=[CH:14][C:13]=2[CH3:18])[N:11]=12.2 g of trichloromethanesulfenyl chloride are introduced into a solution of 2 g of 2,4,6-trimethyl benzamidine in 16 ml of dichloromethane under an inert atmosphere at about -20° C., followed by the slow addition of 2 g of NaOH dissolved in 3.2 ml of water at about -10° C. After I hour at about -5° C., the precipitate formed is isolated and the organic phase is separated and washed with 6 ml of water. After being dried over K2CO3, it is concentrated under reduced pressure to give 2.8 g of the desired product in the form of an oil, which may be used without purification.
読み込み中…
