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Potassium Carbonate → Hexafluoroacetone monohydrate

HRID 1818093
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HRID 1818093 반응식
[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]
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 24408BromineHCID 23683893Potassium 3,3,3-trifluoro-2-trifluoromethyl-2-hydroxypropionate

생성물 1

HCID 61525Hexafluoroacetone monohydrate

시약·촉매·용매 1

HCID 962Water용매

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온도
40 °C

실험 절차

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.

후처리

  1. customIn a 50-ml three-necked flask were placed
  2. dissolutionto dissolve the mixture
  3. additionAfter the completion of dropwise addition

출처 및 근거

ORD 기록
ord-fa4d825861df43c48c6512d9c09ec8ed
출처 데이터셋
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07598425B2

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