Methyl Isobutyl Ketone → HCID 86682208, compound

HRID 2408220Notes

Reaction equation

HRID 2408220 reaction equation
[F:1][C:2]([O:10][C:11]([F:20])([F:19])[C:12]([F:18])([F:17])[C:13]([F:16])([F:15])[F:14])([C:6]([F:9])([F:8])[F:7])[C:3]([OH:5])=[O:4].[Cl-].[C:22]1([S+:28]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.C(C(C)=O)C(C)C>ClCCl>[F:1][C:2]([O:10][C:11]([F:19])([F:20])[C:12]([F:18])([F:17])[C:13]([F:14])([F:15])[F:16])([C:6]([F:9])([F:8])[F:7])[C:3]([O-:5])=[O:4].[C:35]1([S+:28]([C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=1

Participants

5

Reactant 3

HCID 7909Methyl Isobutyl KetoneHCID 61343Triphenylsulfonium chlorideHCID 114481Perfluoro-2-methyl-3-oxahexanoic acid

Product 1

HCID 86682208HCID 86682208, compoundYield 35.4%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To 6.6 g (0.02 mol) of 2,3,3,3-tetrafluoro-2-(1,1,2,2,3,3,3-heptafluoropropoxy)propionic acid were added an amount (0.03 mol) of triphenylsulfonium chloride aqueous solution, 60 g of methyl isobutyl ketone, and 25 g of dichloromethane. An organic layer was taken out, and washed with 50 g of water three times. After the solvent was distilled off in vacuum, the residue was added to diisopropyl ether for crystallization. On filtration and drying, 4.2 g of white crystals was obtained (yield 35%). The compound thus obtained was analyzed by spectroscopy.

Workup

  1. washwashed with 50 g of water three times
  2. distillationAfter the solvent was distilled off in vacuum
  3. additionthe residue was added to diisopropyl ether for crystallization
  4. filtrationOn filtration
  5. customdrying

Sources & evidence

ORD record
ord-7365501878884c4a9c5f5a2828aa7311
Source dataset
uspto-grants-2014_08
Patent number
US08815492B2

Reaction notes

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