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Hydrochloric Acid → 1,1,1-Trifluoro-2-methyl-2-heptanol

HRID 424321
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HRID 424321 반응식
C[Si](C)(C)[C:3]([F:6])([F:5])[F:4].[CH3:9][C:10](=[O:16])[CH2:11][CH2:12][CH2:13][CH2:14][CH3:15].Cl>O.O.O.[F-].C([N+](CCCC)(CCCC)CCCC)CCC.O1CCCC1>[F:4][C:3]([F:6])([F:5])[C:10]([CH3:9])([OH:16])[CH2:11][CH2:12][CH2:13][CH2:14][CH3:15]
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 80512-HeptanoneHCID 552549(Trifluoromethyl)trimethylsilane

생성물 1

HCID 805587151,1,1-Trifluoro-2-methyl-2-heptanol수율 102.3%

시약·촉매·용매 2

HCID 11726816Tetrabutylammonium Fluoride Trihydrate촉매HCID 8028Tetrahydrofuran
용매

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온도
48 °C

실험 절차

24.9 g of trimethyl(trifluoromethyl)silane, 16.0 g of 2-heptanone, 38 g of tetrahydrofuran and 350 mg of tetrabutylammonium fluoride trihydrate were charged into a four-necked flask equipped with a nitrogen feeding tube, a reflux condenser, a dropping funnel and a thermometer, and a reaction was effected by a conventional method. Then, 17.5 g of hydrochloric acid was dropwise added to the reaction mixture at a temperature of 25 to 48° C. over 30 minutes, followed by stirring at about 48° C. for 2 hours. The reaction mixture was treated by a conventional method, and the resulting organic phase was washed with a saline solution, followed by drying with anhydrous magnesium sulfate. Thereafter, the resultant was concentrated under reduced pressure, thereby obtaining 26.4 g of 1,1,1-trifluoro-2-methyl-2-heptanol in the form of a pale brown oily matter.

후처리

  1. customequipped with a nitrogen feeding tube, a reflux condenser, a dropping funnel
  2. additionThe reaction mixture was treated by a conventional method
  3. washthe resulting organic phase was washed with a saline solution
  4. dry with materialby drying with anhydrous magnesium sulfate
  5. concentrationThereafter, the resultant was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-4b5604515fcc4a999830feb3f1db4cea
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08105747B2

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