Hydrochloric Acid → 2-Octanone, 1,1,1-trifluoro-

HRID 2073421노트

반응식

HRID 2073421 반응식
[Mg].[CH2:2](Br)[CH2:3][CH2:4][CH2:5][CH2:6][CH3:7].[F:9][C:10]([F:15])([F:14])[C:11](O)=[O:12].Cl>CCOCC>[F:9][C:10]([F:15])([F:14])[C:11](=[O:12])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6422Trifluoroacetic acidHCID 81011-BromohexaneHCID 5462224Magnesium

생성물 1

HCID 959112-Octanone, 1,1,1-trifluoro-수율 54%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매3회

실험 절차

In a nitrogen atmosphere, 9.12 g (380 mM) of magnesium into 120 ml of ether, and 59.4 g (360 mM) of hexyl bromide dissolved in 30 ml of ether was added thereto, followed by 1.5 hours of heat refluxing. After cooling by standing and with ice, 13.68 g (120 mM) of trifluoroacetic acid dissolved in 30 ml of ether was added. After being stirred for 7 hours under cooling with ice, the system was subjected to hydrolysis with addition of hydrochloric acid, followed by extraction with ether and drying of the resultant ether layer with anhydrous sodium sulfate. The dried product was distilled under normal pressure to obtain 11.8 g of 1,1,1-trifluoro-2-octanone. Yield: 46%.

후처리

  1. additionwas added
  2. temperatureof heat
  3. temperaturerefluxing
  4. temperatureAfter cooling
  5. additionwas added
  6. temperatureunder cooling with ice
  7. extractionfollowed by extraction with ether
  8. dry with materialdrying of the resultant ether layer with anhydrous sodium sulfate
  9. distillationThe dried product was distilled under normal pressure

출처 및 근거

ORD 기록
ord-ccf0ce45b8d243fba9b886fc98cc8ecd
출처 데이터셋
uspto-grants-1990_04
특허 번호
US04917817

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