Sodium Carbonate → Hexafluoroacetone monohydrate

Temperature

40 °C

In a 50-ml three-necked flask were placed 20 mmol of the aqueous sodium 3,3,3-trifluoro-2-trifluoromethyl-2-hydroxypropionate solution prepared in Reference Example 2 and 2.12 g (20 mmol) of sodium carbonate. 20 g of water was added to dissolve the mixture. The pH was 9.8. A reaction was performed by blowing chlorine gas at 20 ml/min for 29 minutes (24.1 mmol, 1.2 eq.) while stirring the solution under heat at 40° C. in a water bath. The pH during this treatment was 6.9. To this solution, 1.06 g (10 mmol) of sodium carbonate was further added, followed by dissolving. The pH was 9.1. The reaction was further performed by blowing chlorine gas at 10 ml/min for 22 minutes (9.2 mmol, 0.46 eq.) while stirring the solution under heat at 40° C. The pH when the reaction was complete was 6.8. Hexafluoroacetone hydrate was obtained at a starting material conversion of 82% with a selectivity of at least 99%.

1. customIn a 50-ml three-necked flask were placed
2. dissolutionto dissolve the mixture
3. customfor 29 minutes
4. dissolutionby dissolving
5. customfor 22 minutes
6. stirringwhile stirring the solution
7. temperatureunder heat at 40° C

ORD record

ord-7a042f50883d4683a301d16256fa33e0

Source dataset

uspto-grants-2009_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07598425B2