Sodium hexafluoroantimonate → HCID 19877071、化合物
反応式
F[B-](F)(F)F.[Cl:6][C:7]1[CH:28]=[CH:27][C:10]([CH2:11][S+:12]([CH2:19][C:20]2[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][CH:21]=2)C2C=CC=CC=2)=[CH:9][CH:8]=1.[F:29][Sb-:30]([F:35])([F:34])([F:33])([F:32])[F:31].[Na+]>C(Cl)Cl>[F:29][Sb-:30]([F:35])([F:34])([F:33])([F:32])[F:31].[Cl:6][C:7]1[CH:28]=[CH:27][C:10]([CH2:11][S+:12]([CH2:19][C:20]2[CH:21]=[CH:22][C:23]([Cl:26])=[CH:24][CH:25]=2)[CH2:11][C:10]2[CH:27]=[CH:28][CH:7]=[CH:8][CH:9]=2)=[CH:9][CH:8]=1参加物
4
実験手順
A mixture of 7.0 g (15.2 mmol) of di-(4-chlorobenzyl)-phenylsulfonium tetrafluoroborate and 25 ml of methylene chloride is dissolved under N2 in a 100 ml round-bottomed flask to give a clear solution and the solution is cooled to 0°-5° C. 5.9 g (22.8 mmol) of sodium hexafluoroantimonate are added at this temperature and the mixture is stirred for about 3 h. The reaction mixture is filtered and the filtrate is freed from the solvent on a rotary evaporator. 50 ml of deionized water are now added to the residue and the product is crystallized out. It is left to crystallize at 0°-5° C. for 1-2 h. The crystals now obtained by filtration are washed with water and dried under a high vacuum at RT overnight. 8.26 g of di-(4-chlorobenzyl)-benzylsulfonium hexafluoroantimonate are obtained as white crystals of melting point 75°-77° C.