Sodium hexafluoroantimonate → HCID 19877071, compound

HRID 1886132Notes

Reaction equation

HRID 1886132 reaction equation
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

Participants

4

Reactant 2

HCID 16689647Sodium hexafluoroantimonateHCID 19795282HCID 19795282, compound

Product 1

HCID 19877071HCID 19877071, compoundYield 178.1%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

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.

Workup

  1. dissolutionis dissolved under N2 in a 100 ml round-bottomed flask
  2. customto give a clear solution
  3. temperaturethe solution is cooled to 0°-5° C
  4. filtrationThe reaction mixture is filtered
  5. customthe filtrate is freed from the solvent on a rotary evaporator
  6. addition50 ml of deionized water are now added to the residue
  7. customthe product is crystallized out
  8. waitIt is left
  9. customto crystallize at 0°-5° C. for 1-2 h
  10. customThe crystals now obtained by filtration
  11. washare washed with water
  12. customdried under a high vacuum at RT overnight

Sources & evidence

ORD record
ord-56fb04b998dc43ce8da967bd102a9f07
Source dataset
uspto-grants-1992_09
Patent number
US05149767

Reaction notes

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