Methane → HCID 19734745, compound

HRID 1886128Notes

Reaction equation

HRID 1886128 reaction equation
S([O-])(O)(=O)=O.[CH2:6]([S+:13]([CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[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:28][Sb-:29]([F:34])([F:33])([F:32])([F:31])[F:30].[Na+].C>CO>[F:28][Sb-:29]([F:34])([F:33])([F:32])([F:31])[F:30].[CH2:21]([S+:13]([CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[CH2:14][C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1)[C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1

Participants

5

Reactant 3

HCID 297MethaneHCID 16689647Sodium hexafluoroantimonateHCID 21653994HCID 21653994, compound

Product 1

HCID 19734745HCID 19734745, compoundYield 74%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

16.64 g (0.041 mol) of tribenzylsulfonium hydrogen sulfate are dissolved in 750 ml of hot methanol. 16.04 g (0.062 mol) of solid sodium hexafluoroantimonate are added to the cloudy solution and the mixture is stirred at RT for 1 h. After addition of 1 spatula-full of active charcoal, the mixture is filtered and 750 ml of water are added to the clear filtrate. The crystals which have precipitated are filtered off, dried, washed with 100 ml of ether and dried again. 16.41 g (74% of theory) of tribenzylsulfonium hexafluoroantimonate are obtained as colourless crystals of melting point 170° C. (decomposition).

Workup

  1. filtrationthe mixture is filtered
  2. addition750 ml of water are added to the clear filtrate
  3. customThe crystals which have precipitated
  4. filtrationare filtered off
  5. customdried
  6. washwashed with 100 ml of ether
  7. customdried again

Sources & evidence

ORD record
ord-c4a427ff18f14e458ca879412bd0cf43
Source dataset
uspto-grants-1992_09
Patent number
US05149767

Reaction notes

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