Water → HCID 21470465, compound

HRID 2294753Notes

Reaction equation

HRID 2294753 reaction equation
ClC1C=CC=C(C(OO)=[O:9])C=1.O.[F:13][C:14]([F:27])([F:26])[C:15]([C:22]([F:25])([F:24])[F:23])([C:18]([F:21])([F:20])[F:19])[CH:16]=[CH2:17].C(=O)(O)[O-].[Na+]>C(OCC)C>[F:13][C:14]([F:26])([F:27])[C:15]([C:18]([F:21])([F:20])[F:19])([C:22]([F:23])([F:24])[F:25])[CH:16]1[O:9][CH2:17]1

Participants

6

Reactant 4

HCID 962WaterHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 278262914115-46-9

Product 1

HCID 21470465HCID 21470465, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

32.9 g (105 mmol) of 3-chloroperbenzoic acid with a peracid content of 55% is added in portions with stirring and cooling with water to a solution of 24.6 g (100 mmol) of 4,4,4-trifluoro-3,3-bis(trifluoromethyl)-but-1-ene in 150 ml of absolute diethyl ether. After addition is completed, it is refluxed for 3 hours. It is allowed to cool, and the solution is stirred in cold, saturated sodium bicarbonate solution. The ethereal solution is separated, washed with sodium chloride solution, dried on sodium sulfate and concentrated by evaporation on a column. The residue is purified by bulb tube distillation (vacuum 30 mbar, 130° C. bath).

Workup

  1. additionAfter addition
  2. temperatureit is refluxed for 3 hours
  3. temperatureto cool
  4. customThe ethereal solution is separated
  5. washwashed with sodium chloride solution
  6. customdried on sodium sulfate
  7. concentrationconcentrated by evaporation on a column
  8. customThe residue is purified by bulb tube
  9. distillationdistillation (vacuum 30 mbar, 130° C. bath)

Sources & evidence

ORD record
ord-9913ec651e9f423a947bb83c71eef2ac
Source dataset
uspto-grants-1997_11
Patent number
US05690909

Reaction notes

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