Sodium hexafluoroantimonate → Dibenzyl(phenyl)sulfanium hexafluoroantimonate(1-)

HRID 1886130ノート

反応式

HRID 1886130 の反応式
F[B-](F)(F)F.[CH2:6]([SH+:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[F:21][Sb-:22]([F:27])([F:26])([F:25])([F:24])[F:23].[Na+]>C(Cl)Cl>[F:21][Sb-:22]([F:27])([F:26])([F:25])([F:24])[F:23].[CH2:14]([S+:13]([CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

参加物

4

反応物 2

HCID 16689647Sodium hexafluoroantimonateHCID 19877065HCID 19877065、化合物

生成物 1

HCID 21263248Dibenzyl(phenyl)sulfanium hexafluoroantimonate(1-)収率 191.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 123.0 g (0.325 mol) of dibenzylsulfonium tetrafluoroborate in 400 ml of methylene chloride is dissolved in a 2 liter round-bottomed flask at RT under N2 to give a clear solution. 117.8 g of sodium hexafluoroantimonate are then added and the mixture is stirred at RT for 31/2 h. The suspension is now filtered over silica gel and the solvent is removed from the filtrate using a rotary evaporator. The slightly reddish viscous residue is dissolved again in 250 ml of methanol, and after addition of 250 ml of water the product is allowed to crystallize at RT for 1-2 h. The suspension is filtered and the residue is washed with water. The product is then dried under a high vacuum at RT overnight. 163.9 g (95% of theory) of dibenzylphenylsulfonium hexafluoroantimonate are obtained as white crystals of melting point 105°-109° C.

後処理

  1. dissolutionis dissolved in a 2 liter round-bottomed flask at RT under N2
  2. customto give a clear solution
  3. filtrationThe suspension is now filtered over silica gel
  4. customthe solvent is removed from the filtrate
  5. customa rotary evaporator
  6. dissolutionThe slightly reddish viscous residue is dissolved again in 250 ml of methanol
  7. additionafter addition of 250 ml of water the product
  8. customto crystallize at RT for 1-2 h
  9. filtrationThe suspension is filtered
  10. washthe residue is washed with water
  11. customThe product is then dried under a high vacuum at RT overnight

出典と根拠

ORDレコード
ord-758fbc23794545e98acc52c60347c6e6
出典データセット
uspto-grants-1992_09
特許番号
US05149767

反応ノート

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