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Halothane → 1,1,1-Trifluoro-2-bromo-2-chloro-5-methyl-4-hexen-3-ol

HRID 3013
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HRID 3013 반응식
CC(C)([O-])C.[Na+].[Br:7][CH:8]([Cl:13])[C:9]([F:12])([F:11])[F:10].[CH:14](=[O:19])[CH:15]=[C:16]([CH3:18])[CH3:17]>O1CCCC1>[Br:7][C:8]([Cl:13])([C:9]([F:12])([F:11])[F:10])[CH:14]([OH:19])[CH:15]=[C:16]([CH3:18])[CH3:17]
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참가 물질

5

반응물 3

HCID 3562HalothaneHCID 610203-Methyl-2-butenalHCID 23676156Sodium t-butoxide

생성물 1

HCID 152193461,1,1-Trifluoro-2-bromo-2-chloro-5-methyl-4-hexen-3-ol수율 73.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
-60 °C

실험 절차

Tetrahydrofuran (230 ml) and sodium t-butoxide (57.6 g; 40% w/v solution in dimethylformamide) was charged to a split-neck reaction flask, and cooled to -60° C. with stirring. 1-Bromo-1-chloro-2,2,2-trifluorethane (47.6 g) and senecialdehyde (20.9 g) were charged simultaneously over 25 minutes, then the mixture was stirred at -60° C. for a further 30 minutes. On completion of reaction, the mass was quenched by controlled addition of saturated ammonium chloride solution (120 ml). Hexane (500 ml) was added to the mixture, then the aqueous phase was separated and extracted with further hexane (2×500 ml). The combined organics were washed with brine (2×100 ml) and then water (3×20 ml). Drying (sodium sulphate) and concentration in vacuo then gave the product 5-bromo-5-chloro-4-hydroxy-2-methyl-6,6,6-trifluorohex-2-ene as a mobile yellow oil (50.1 g, 70% yield).

후처리

  1. stirringthe mixture was stirred at -60° C. for a further 30 minutes
  2. customOn completion of reaction
  3. customthe mass was quenched by controlled addition of saturated ammonium chloride solution (120 ml)
  4. additionHexane (500 ml) was added to the mixture
  5. customthe aqueous phase was separated
  6. extractionextracted with further hexane (2×500 ml)
  7. washThe combined organics were washed with brine (2×100 ml)
  8. customDrying
  9. concentration(sodium sulphate) and concentration in vacuo

출처 및 근거

ORD 기록
ord-c5c150db0d6042c384ac6e15e60907af
출처 데이터셋
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05731475

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