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tert-Butyl methyl ether → 4-Bromo-1-fluoro-2-fluoromethyl-3-butyn-2-yl 4-Trifluoromethylphenyl Ether

HRID 1282434
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HRID 1282434 반응식
[F:1][C:2]([F:18])([F:17])[C:3]1[CH:8]=[CH:7][C:6]([O:9][C:10]([CH2:15][F:16])([C:13]#[CH:14])[CH2:11][F:12])=[CH:5][CH:4]=1.COC(C)(C)C.CC(C)([O-])C.[K+].[Br:31]Br>CCCCCC.C(O)(C)(C)C>[F:1][C:2]([F:17])([F:18])[C:3]1[CH:8]=[CH:7][C:6]([O:9][C:10]([CH2:11][F:12])([C:13]#[C:14][Br:31])[CH2:15][F:16])=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 15413tert-Butyl methyl etherHCID 24408BromineHCID 184244041-Fluoro-2-fluoromethyl-3-butyn-2-yl 4-trifluoromethylphenyl etherHCID 23665647Potassium tert-butoxide

생성물 1

HCID 184244154-Bromo-1-fluoro-2-fluoromethyl-3-butyn-2-yl 4-Trifluoromethylphenyl Ether

시약·촉매·용매 2

HCID 6386
tert-Butanol
용매
HCID 8058Hexane용매

실험 절차

An amount (13.9 g) of 1-fluoro-2-fluoromethyl-3-butyn-2-yl 4-trifluoromethylphenyl ether was dissolved in a solvent consisting of a mixture of tert-butyl methyl ether (100 ml) and tert-butyl alcohol (150 ml). To the solution under cooling with ice, potassium tert-butoxide (7.1 g) was added under a nitrogen atmosphere; after stirring for a while, bromine (3 ml) was added dropwise. After the end of the dropwise addition, the mixture was stirred for 30 minutes under stirring with ice. Hexane was added to the reaction mixture, which was then washed with water and a saturated aqueous solution of sodium chloride. The mixture was dried with anhydrous sodium sulfate and concentrated under reduced pressure to give the titled compound (18.1 g).

후처리

  1. additionwas added under a nitrogen atmosphere
  2. additionwas added dropwise
  3. additionAfter the end of the dropwise addition
  4. stirringunder stirring with ice
  5. washwas then washed with water
  6. dry with materialThe mixture was dried with anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-81847dd3e14447bd8eb9f9c76f73b72c
출처 데이터셋
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06455708B1

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