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Water → 4-(2-Trifluoromethylphenyl)-3-buten-2-one

HRID 9927
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인쇄 미리보기

반응식

HRID 9927 반응식
CON(C)[C:4](=[O:17])[CH:5]=[CH:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[C:13]([F:16])([F:15])[F:14].C[Li].O.[C:22](OCC)(=O)C>O1CCCC1.C(OCC)C>[F:14][C:13]([F:16])([F:15])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=1[CH:6]=[CH:5][C:4](=[O:17])[CH3:22]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 73858026N-methoxy-N-methyl-3-(2-trifluoromethylphenyl)acrylamideHCID 178418348HCID 178418348, 화합물

생성물 1

HCID 5226124-(2-Trifluoromethylphenyl)-3-buten-2-one

시약·촉매·용매 2

HCID 3283Diethyl Ether용매
HCID 8028
Tetrahydrofuran
용매

반응 조건

온도
-78 °C

실험 절차

11 g of N-methoxy-N-methyl-3-(2-trifluoromethylphenyl)acrylamide are dissolved in 150 ml of dry tetrahydrofuran under a nitrogen atmosphere, cooled to −78° C. and treated dropwise with 36 ml of a 1.4N solution of methyllithium in diethyl ether in 10 minutes. The solution is subsequently furthermore stirred at −78° C. for 2 h and then hydrolysed with water. 200 ml of ethyl acetate are now added at ambient temperature and the mixture is washed three times with saturated sodium chloride solution. The organic phase is finally separated, dried with magnesium sulfate and evaporated under reduced pressure. After purifying by flash chromatography, the title compound is thus obtained.

후처리

  1. washthe mixture is washed three times with saturated sodium chloride solution
  2. customThe organic phase is finally separated
  3. dry with materialdried with magnesium sulfate
  4. customevaporated under reduced pressure
  5. customAfter purifying by flash chromatography

출처 및 근거

ORD 기록
ord-b59c10a751ce41438cf1eb1cd9957f87
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07091371B2

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