Potassium Carbonate → Hexafluoroacetone monohydrate
Reaction equation
[F:1][C:2]([F:13])([F:12])[C:3]([C:8]([F:11])([F:10])[F:9])([OH:7])C([O-])=[O:5].[K+].C(=O)([O-])[O-].[K+].[K+].BrBr>O>[OH2:5].[F:1][C:2]([F:13])([F:12])[C:3]([C:8]([F:11])([F:10])[F:9])=[O:7]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 40 °C
Procedure
In a 50-ml three-necked flask were placed 7.59 g (17.2 mmol) of the aqueous 56.8% potassium 3,3,3-trifluoro-2-trifluoromethyl-2-hydroxypropionate solution prepared in Reference Example 1 and 4.98 g (36 mmol) of potassium carbonate. 25 g of water was added to dissolve the mixture. The pH was 13. 5.75 g (36 mmol) of bromine was added dropwise over 60 minutes while stirring the mixture under heat at 40° C. in a water bath. After the completion of dropwise addition, the reaction was further performed at the same temperature for 3 hours, and the reaction was complete. The pH when the reaction was complete was 7 to 8. Hexafluoroacetone hydrate was obtained at a starting material conversion of 64% with a selectivity of 99% or higher.
Workup
- customIn a 50-ml three-necked flask were placed
- dissolutionto dissolve the mixture
- additionAfter the completion of dropwise addition
Sources & evidence
- ORD record
- ord-fa4d825861df43c48c6512d9c09ec8ed
- Source dataset
- uspto-grants-2009_10
- Patent number
- US07598425B2
Reaction notes
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