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1,2-Dibromoethane → [2-[4-(3,3-Dimethoxy-4,4,4-trifluorobut-1-yl)phenoxy]ethyl]bromide

HRID 1700912
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HRID 1700912 반응식
[CH3:1][O:2][C:3]([O:17][CH3:18])([C:13]([F:16])([F:15])[F:14])[CH2:4][CH2:5][C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].[Br:25][CH2:26][CH2:27]Br>>[CH3:18][O:17][C:3]([O:2][CH3:1])([C:13]([F:15])([F:16])[F:14])[CH2:4][CH2:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:27][CH2:26][Br:25])=[CH:8][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 78391,2-DibromoethaneHCID 11430Potassium CarbonateHCID 183189964-(3,3-Dimethoxy-4,4,4-trifluorobut-1-yl)phenol

생성물 1

HCID 18319078[2-[4-(3,3-Dimethoxy-4,4,4-trifluorobut-1-yl)phenoxy]ethyl]bromide수율 86.9%

반응 조건

온도
130 °C

실험 절차

A mixture of 4-(3,3-dimethoxy-4,4,4-trifluorobut-1-yl)phenol (1.64 g, 6.2 mmol), potassium carbonate (1.3 g, 9.3 mmol) and 1,2-dibromoethane (5 ml, 58 mmol) was stirred and heated under reflux (130° C.) for 26 h. After cooling to room temperature, the mixture was filtered and washed with ethyl actate. The filtrate was concentrated in vacuo and the residue was purified by column chromatography (silica gel, hexane/ethyl acetate 20:1 to 4:1) to give the title compound (2.0 g, 85%) as a colorless liquid.

후처리

  1. temperatureheated
  2. temperatureAfter cooling to room temperature
  3. filtrationthe mixture was filtered
  4. washwashed with ethyl actate
  5. concentrationThe filtrate was concentrated in vacuo
  6. customthe residue was purified by column chromatography (silica gel, hexane/ethyl acetate 20:1 to 4:1)

출처 및 근거

ORD 기록
ord-b2342d83240740e78d8429d622f1d9e6
출처 데이터셋
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06350892B1

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