Magnesium perchlorate → 2-Bromo-3-oxo-hexanoic acid ethyl ester

HRID 401597

반응식

HRID 401597 반응식
[CH2:1]([O:3][C:4](=[O:11])[CH2:5][C:6](=[O:10])[CH2:7][CH2:8][CH3:9])[CH3:2].Cl([O-])(=O)(=O)=O.[Mg+2].Cl([O-])(=O)(=O)=O.[Br:23]N1C(=O)CCC1=O>C(OCC)(=O)C.C(OCC)C>[CH2:1]([O:3][C:4](=[O:11])[CH:5]([Br:23])[C:6](=[O:10])[CH2:7][CH2:8][CH3:9])[CH3:2]

참가 물질

6

반응물 3

HCID 24840Magnesium perchlorateHCID 67184N-bromobutanimideHCID 238498Ethyl 3-oxohexanoate

생성물 1

HCID 130155942-Bromo-3-oxo-hexanoic acid ethyl ester

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8857Ethyl Acetate용매2회

실험 절차

3-Oxo-hexanoic acid ethyl ester (4.0 mL, 25 mmol) and magnesium perchlorate (1.7 g, 7.6 mmol) were placed in 500 mL of ethyl acetate and allowed to stir for 5 minutes. N-Bromosuccinimide (4.7 g, 26 mmol) was added and the reaction mixture was allowed to stir for 15 minutes, at which time thin-layer chromatography (10% ethyl acetate in hexanes, silica gel, 254 nm irradiation) indicated the reaction was complete. The reaction mixture was diluted with 500 mL of ethyl ether and washed three times with an equal volume of saturated aqueous sodium chloride. The organic layer was then dried over sodium sulfate and evaporated to dryness. This material was used in the next step without further purification.

후처리

  1. washwashed three times with an equal volume of saturated aqueous sodium chloride
  2. dry with materialThe organic layer was then dried over sodium sulfate
  3. customevaporated to dryness
  4. customThis material was used in the next step without further purification

출처 및 근거

ORD 기록
ord-e9222980ba39455cb6073d6bb32e4d1b
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08741939B2

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