Hydrogen Peroxide → HCID 86700528, compound

HRID 625189Notes

Reaction equation

HRID 625189 reaction equation
[CH3:1][O:2][C:3]([CH:5]1[CH2:9][CH:8]([C:10]([O:12][CH3:13])=[O:11])[CH2:7][CH:6]1[C:14]([F:22])([F:21])[C:15]([F:20])([F:19])[S:16]([O-:18])=[O:17])=[O:4].[Na+:23].[OH:24]O>[O-][W]([O-])(=O)=O.[Na+].[Na+].O>[CH3:1][O:2][C:3]([CH:5]1[CH2:9][CH:8]([C:10]([O:12][CH3:13])=[O:11])[CH2:7][CH:6]1[C:14]([F:22])([F:21])[C:15]([F:19])([F:20])[S:16]([O-:24])(=[O:18])=[O:17])=[O:4].[Na+:23]

Participants

5

Procedure

Into a glass flask equipped with a thermometer and a capacitor were charged the aqueous solution of crude sodium 2-(2,4-bis(methoxycarbonyl)cyclopentyl)-1,1,2,2-tetrafluoroethanesulfinate obtained as described above, and a catalytic amount of sodium tungstate (IV) dihydrate. Thereto, a 35% by mass hydrogen peroxide solution 3.00 g was added dropwise. After the mixture was stirred at room temperature for 5 hrs, the disappearance of the raw material was confirmed by 19F-NMR to decide completion of the reaction. After the completion of the reaction, 20 mL of water was further added thereto, and the aqueous layer was washed with 30 mL of dichloromethane five times to obtain an aqueous solution of sodium 2-(2,4-bis(methoxycarbonyl)cyclopentyl)-1,1,2,2-tetrafluoroethanesulfonate (precursor compound (a-5)) represented by the following formula (a-5), which was used for the following reaction.

Workup

  1. customInto a glass flask equipped with a thermometer
  2. customobtained
  3. customcompletion of the reaction
  4. additionwas further added
  5. washthe aqueous layer was washed with 30 mL of dichloromethane five times

Sources & evidence

ORD record
ord-b99f3bb37e664cd6b36133c4319e30fb
Source dataset
uspto-grants-2016_04
Patent number
US09304393B2

Reaction notes

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