Water → HCID 13850776、化合物

反応式

[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10][N:11]([CH2:15][CH2:16][OH:17])[CH2:12][CH2:13][OH:14])([O-:3])=[O:2].[C:18]1([CH3:28])[CH:23]=[CH:22][C:21]([S:24](Cl)(=[O:26])=[O:25])=[CH:20][CH:19]=1.[OH2:29]>N1C=CC=CC=1>[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10][N:11]([CH2:15][CH2:16][O:17][S:24]([C:21]1[CH:22]=[CH:23][C:18]([CH3:28])=[CH:19][CH:20]=1)(=[O:25])=[O:29])[CH2:12][CH2:13][O:14][S:24]([C:21]1[CH:22]=[CH:23][C:18]([CH3:28])=[CH:19][CH:20]=1)(=[O:26])=[O:25])([O-:3])=[O:2]

参加物

実験手順

389 g (1.5 mol) of crude N-(2-nitrophenylsulphenyl)-bis(2-hydroxyethyl)-amine are dissolved in 2 l of absolute pyridine, and 580 g (3 mol) of 4-toluenesulphonyl chloride are added at -10° in the course of 20 minutes. The mixture is stirred at -5° to 0° for 4 hours and left to stand at 0° overnight, and 4 l of water are added. Thereafter, the mixture is extracted with 3×1 l of methylene chloride and the extract is washed with 7×1 l of water, dried with sodium sulphate and concentrated. The oily residue is stirred with 1 l of a mixture of acetonitrile/methanol (1:1), a solid product precipitating, which is filtered off with suction with methanol. Yield: 423.6 g of melting point 91°-93°.