Sulfuric Acid → Hexafluoroacetylacetone

HRID 1266683Notes

Reaction equation

HRID 1266683 reaction equation
[CH2:1]([C:9](O)([OH:14])[C:10]([F:13])([F:12])[F:11])[C:2](O)([OH:7])[C:3]([F:6])([F:5])[F:4].S(=O)(=O)(O)O>>[CH2:1]([C:2]([C:3]([F:4])([F:5])[F:6])=[O:7])[C:9]([C:10]([F:11])([F:13])[F:12])=[O:14]

Participants

3

Reactant 2

HCID 1118Sulfuric AcidHCID 1441991,1,1,5,5,5-Hexafluoro-2,2,4,4-pentane-t etrol, 97

Product 1

HCID 73706HexafluoroacetylacetoneYield 90.5%

Procedure

A 100-ml eggplant-type flask was charged with 16.2 g of the obtained 1,1,1,5,5,5-hexafluoroacetylacetone dihydrate and 33.0 g of 98% sulfuric acid. Then, the flask was stopped, and the mixture was stirred for 4 hr at room temperature with a magnetic mixer, followed by standing still for 1 hr to have two layers separated from each other. Then, 12.5 g of 1,1,1,5,5,5-hexafluoroacetylacetone were obtained from the organic layer. This product was found by a gas chromatography (detector: FED, column: DB-1, column size: 0.25 mm×60 m) to be 1,1,1,5,5,5-hexafluoroacetylacetone having a purity of 99.9% (areal % in gas chromatography).

Workup

  1. waitby standing still for 1 hr
  2. customseparated from each other

Sources & evidence

ORD record
ord-4205e6b0565b40aaba4f609d1dde2f8f
Source dataset
uspto-grants-2003_04
Patent number
US06548712B2

Reaction notes

Loading…