Benzyl Alcohol → Benzyl 4,4-dimethoxy-3-oxobutyrate

HRID 1700335

반응식

HRID 1700335 반응식
[CH3:1][O:2][CH:3]([O:12][CH3:13])[C:4](=[O:11])[CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7].C(O)[C:15]1[CH:20]=[CH:19]C=[CH:17][CH:16]=1.P([O-])([O-])([O-])=O>CN(C)C1C=CN=CC=1.C1(C)C=CC=CC=1>[CH3:1][O:2][CH:3]([O:12][CH3:13])[C:4](=[O:11])[CH2:5][C:6]([O:8][CH2:9][C:10]1[CH:19]=[CH:20][CH:15]=[CH:16][CH:17]=1)=[O:7]

참가 물질

6

반응물 3

HCID 244Benzyl AlcoholHCID 1061PhosphateHCID 248327Ethyl 4,4-dimethoxy-3-oxobutanoate

생성물 1

HCID 18318278Benzyl 4,4-dimethoxy-3-oxobutyrate

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 1140Toluene용매

실험 절차

2.68 g (14.1 mmol) of ethyl 4,4-dimethoxy-3-oxo-butyrate, 3.62 ml (34.9 mmol) of benzyl alcohol and 244 mg (2.0 mmol) of 4-dimethylaminopyridine were heated under reflux in 40 ml of toluene for three nights. A phosphate buffer solution was added to the obtained reaction solution. After the extraction with ethyl acetate, the organic layer was washed with a saturated aqueous salt solution and then dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by the silica gel chromatography (hexane/ethyl acetate=9:1) to obtain the title compound.

후처리

  1. extractionAfter the extraction with ethyl acetate
  2. washthe organic layer was washed with a saturated aqueous salt solution
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by the silica gel chromatography (hexane/ethyl acetate=9:1)

출처 및 근거

ORD 기록
ord-5528c3d14ce94083a61c9fa6555a229c
출처 데이터셋
uspto-grants-2002_02
특허 번호
US06350762B1

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