Chlorobenzene → Benzene, 1,1'-sulfonylbis-, dichloro deriv.
反応式
Cl[S:2]([OH:5])(=O)=[O:3].S(Cl)(Cl)=O.[Cl:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>>[CH:15]1[CH:16]=[C:11]([Cl:10])[CH:12]=[C:13]([S:2]([C:13]2[CH:14]=[CH:15][CH:16]=[C:11]([Cl:10])[CH:12]=2)(=[O:5])=[O:3])[CH:14]=1参加物
4
反応条件
- 温度
- 195 °C
実験手順
The filtrate from Example 1 is freed from methoanol by distillation, the residue is returned to the reaction vessel, and 562.5 g (5 mol) of chlorobenzene is added. chlorobenzenesulfonic acid chloride is formed by adding 476 g (4 mol) of chlorosulfonic acid and 466 g (4 mol) of thionyl chloride, the mixture is heated to 195° C., and 337.5 g (3 mol) of chlorobenzene is added at such a rate that the temperature does not fall. the charge is subsequently treated as described in Example 1, giving 850 g (74% yield) of dichlorodiphenyl sulfone of melting point 149°-150° C. Gas-chromatographic analysis of the product gives 99.6% 4,4'-isomer, 0.3% 2,4'-isomer, and 0.1% 3,4'-isomer.