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Ethyl bromoacetate → (2-Bromo-4-trifluoromethyl-phenoxy)-acetic acid ethyl ester

HRID 898584
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반응식

HRID 898584 반응식
[Br:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[CH:4][C:3]=1[OH:12].Br[CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16]>CCN(C(C)C)C(C)C.CCOC(C)=O>[Br:1][C:2]1[CH:7]=[C:6]([C:8]([F:10])([F:11])[F:9])[CH:5]=[CH:4][C:3]=1[O:12][CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 7748Ethyl bromoacetateHCID 27611682-Bromo-4-(trifluoromethyl)phenol

생성물 1

HCID 85969223(2-Bromo-4-trifluoromethyl-phenoxy)-acetic acid ethyl ester

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 81531Diisopropylethylamine용매

실험 절차

A solution of 2.650 g (11.000 mmol) 2-bromo-4-trifluoromethyl-phenol and 1.47 mL 13.20 mmol) ethyl bromo-acetate in 20 mL Hünig base was stirred for 5 h at 120° C. The reaction mixture was diluted with EtOAc and the org. phase was washed with water, saturated aqueous sodium bicarbonate and saturated aqueous NaCl, dried over magnesium sulphate and evaporated down i. vac. Column chromatography (silica gel, gradient dichloromethane/MeOH 100:0→19:1) yielded the product.

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후처리

  1. washphase was washed with water, saturated aqueous sodium bicarbonate and saturated aqueous NaCl
  2. dry with materialdried over magnesium sulphate
  3. customevaporated down i
  4. customColumn chromatography (silica gel, gradient dichloromethane/MeOH 100:0→19:1) yielded the product

출처 및 근거

ORD 기록
ord-b0f172d4b6874120b10e0f4653046180
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07351719B2

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