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Ethyl Acetate → HCID 15922633, 화합물

HRID 1836171
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HRID 1836171 반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:13])=[C:6]([C:8]([CH3:12])([CH3:11])[C:9]#N)[CH:7]=1.[H-].C([Al+]CC(C)C)C(C)C.C(OCC)(=[O:26])C>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:13])=[C:6]([C:8]([CH3:12])([CH3:11])[CH:9]=[O:26])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 15922632HCID 15922632, 화합물HCID 21225700Diisobutylaluminumhydride

생성물 1

HCID 15922633HCID 15922633, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

6.1 g of 2-(5-fluoro-2-methylphenyl)-2-methylpropionitrile, dissolved in 60 ml of toluene, is mixed at −70° C. for 45 minutes with 44 ml of 1.2 M diisobutylaluminum hydride solution in toluene. After 4 hours at −78° C., 120 ml of ethyl acetate is added in drops. It is heated to room temperature and washed three times with 2N sulfuric acid and once with water. The ethyl acetate phase is dried (Na2SO4) and concentrated by evaporation. After distillation, 5.3 g of 2-(5-fluoro-2-methylphenyl)-2-methylpropionaldehyde of boiling point 120° C./0.031 hPa is obtained.

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후처리

  1. washwashed three times with 2N sulfuric acid
  2. dry with materialThe ethyl acetate phase is dried (Na2SO4)
  3. concentrationconcentrated by evaporation
  4. distillationAfter distillation, 5.3 g of 2-(5-fluoro-2-methylphenyl)-2-methylpropionaldehyde of boiling point 120° C./0.031 hPa
  5. customis obtained

출처 및 근거

ORD 기록
ord-5eca6c8eff8b486b8f0eaaf1b7eeadb5
출처 데이터셋
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06777409B2

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