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Hydrogen Bromide → 5-Bromo-2,2-difluoropentanoic acid

HRID 1249532
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HRID 1249532 반응식
Br.[Br:2][CH2:3][CH2:4][CH2:5][C:6]([F:12])([F:11])[C:7]([O:9]C)=[O:8].CCOCC>O>[Br:2][CH2:3][CH2:4][CH2:5][C:6]([F:12])([F:11])[C:7]([OH:9])=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 260Hydrogen Bromide3회HCID 3283Diethyl EtherHCID 13769950Methyl 5-bromo-2,2-difluoropentanoate

생성물 1

HCID 137699515-Bromo-2,2-difluoropentanoic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

HBr gas was introduced into 48% HBr in H2O (100 ml) with occasional cooling in an ice bath until the weight became 180 g. The HBr solution was then added to Part (5) compound (8.4 g, 36.3 mmole) at room temperature and the reaction was stirred for 5 hours at room temperature. The reaction was cooled to 0° C. and poured into Et2O (900 ml) in an ice bath. The products were extracted into the Et2O layer. The water layer was further extracted with Et2O (200 ml and 100 ml). The combined ether layers were washed with H2O (200 ml). The H2O wash was backwashed with Et2O (100 ml). The Et2O layers were combined and dried over MgSO4. Filtration and evaporation of solvent gave the title compound (7.8 g, quant.) as a colorless liquid.

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후처리

  1. temperaturewith occasional cooling in an ice bath until the weight
  2. temperatureThe reaction was cooled to 0° C.
  3. extractionThe products were extracted into the Et2O layer
  4. extractionThe water layer was further extracted with Et2O (200 ml and 100 ml)
  5. washThe combined ether layers were washed with H2O (200 ml)
  6. washThe H2O wash
  7. dry with materialdried over MgSO4
  8. filtrationFiltration and evaporation of solvent

출처 및 근거

ORD 기록
ord-a430d0cba0e14f8ca42afa1c0278414b
출처 데이터셋
uspto-grants-1986_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04632931

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