Dimethyl Sulfide → Hexafluoroacetone trihydrate

HRID 534711Notes

Reaction equation

HRID 534711 reaction equation
C[O:2]C1(F)O[C:6]([C:12]([F:15])([F:14])[F:13])([C:8]([F:11])([F:10])[F:9])[O:5]O1.CSC>[Cl-].[Na+].O>[OH2:2].[OH2:2].[OH2:2].[F:9][C:8]([F:11])([F:10])[C:6]([C:12]([F:15])([F:14])[F:13])=[O:5]

Participants

4

Reactant 2

HCID 1068Dimethyl SulfideHCID 71724327HCID 71724327, compound

Product 1

HCID 36719Hexafluoroacetone trihydrateYield 264.8%

Reagents, catalysts & solvents 1

HCID 57417360Sodium chloride; waterSolvent

Conditions

Temperature
0 °C

Procedure

100 g (0.38 mol) of 1-fluoro-4,4-bis(trifluoromethyl)-2,3,5-trioxolanyl methyl ether (purity: 98%) was charged in a 500-ml five-necked flask. While performing nitrogen bubbling, brine at −20° C. was passed through a Dimroth condenser. While stirring at a reaction temperature of −20° C., 23.4 g (0.38 mol) of dimethyl sulfide was added dropwise using a dropping funnel over 30 minutes. The gas obtained by the reaction was collected by a water trap cooled with ice water to 0° C., and the obtained aqueous layer was analyzed by 19F-NMR. As a result, it was confirmed that 73.8 g (yield: 89%) of hexafluoroacetone trihydrate was obtained.

Workup

  1. customat −20° C.
  2. additionwas added dropwise
  3. customover 30 minutes
  4. customThe gas obtained by the reaction
  5. customwas collected by a water trap

Sources & evidence

ORD record
ord-bb9cfd311a894b5aafe7f9f2d22d5815
Source dataset
uspto-grants-2014_10
Patent number
US08853462B2

Reaction notes

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