Triphenylsulfonium Bromide → Triphenylsulfonium 1,1-difluoro-2-(2-methyl-acryloyloxy)-ethane-1-sulfonate
반응식
[F:1][C:2]([F:14])([S:10]([O-:13])(=[O:12])=[O:11])[CH2:3][O:4][C:5](=[O:9])[C:6]([CH3:8])=[CH2:7].C([NH+](CC)CC)C.[Br-].[C:23]1([S+:29]([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>C(Cl)(Cl)Cl>[F:14][C:2]([F:1])([S:10]([O-:13])(=[O:12])=[O:11])[CH2:3][O:4][C:5](=[O:9])[C:6]([CH3:8])=[CH2:7].[C:36]1([S+:29]([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=2)[C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=1참가 물질
4
실험 절차
A 50 mL reactor was charged with the triethylammonium 1,1-difluoro-2-(2-methyl-acryloyloxy)-ethane-1-sulfonate aqueous solution obtained by the 3rd step, and a solution of 3.18 g (8.9 millimoles) of triphenylsulfonium bromide and 20 g of chloroform, followed by 3 hours of stirring at room temperature. Subsequently, an organic layer was separated, and the thus obtained organic layer was rinsed with 20 g of water four times. Subsequently, it was rinsed with 20 g of diisopropyl ether three times and then a volatile component was distilled off, thereby obtaining 3.92 g of a target triphenylsulfonium 1,1-difluoro-2-(2-methyl-acryloyloxy)-ethane-1-sulfonate. It exhibited a purity of 97% at this time, and a yield of 87% taken over from the 3rd step.