Methanol → HCID 14404104、化合物
反応式
S(Cl)(Cl)=O.[C:5]([C:8]1[CH:13]=[CH:12][C:11]([S:14]([CH2:17][N+:18]([O-:20])=[O:19])(=[O:16])=[O:15])=[CH:10][CH:9]=1)([OH:7])=[O:6].[CH3:21]O>>[CH3:21][O:6][C:5]([C:8]1[CH:9]=[CH:10][C:11]([S:14]([CH2:17][N+:18]([O-:20])=[O:19])(=[O:15])=[O:16])=[CH:12][CH:13]=1)=[O:7]参加物
4
実験手順
Thionyl chloride (0.33 ml, 4.5 mmol) was added dropwise to a stirred solution of (4-carboxyphenylsulphonyl)nitromethane (1.0 g, 4 mmol) in methanol (12 ml) cooled in an ice-salt bath. The mixture was stirred for 16 hours at ambient temperature and the solvent evaporated. The residue was purified by MPLC eluting with dichloromethane, gradually increasing to methanol/dichloromethane (1:50 v/v), to give (4-methoxycarbonylphenylsulphonyl)nitromethane (0.45 g), m.p. 106°-108° C.; microanalysis, found: C, 41.8; H, 3.5; N, 5.2%; C9H9NO6S requires: C, 41.7; H, 3.5: N, 5.4%.
後処理
- temperaturecooled in an ice-salt bath