Ethyl 2,4-dioxovalerate → Ethyl 2-(methoxyimino)-4-oxopentanoate

HRID 251947

반응식

HRID 251947 반응식
O=[C:2]([CH2:8][C:9](=[O:11])[CH3:10])[C:3]([O:5][CH2:6][CH3:7])=[O:4].Cl.[CH3:13][O:14][NH2:15]>C(O)C>[CH3:13][O:14][N:15]=[C:2]([CH2:8][C:9](=[O:11])[CH3:10])[C:3]([O:5][CH2:6][CH3:7])=[O:4]

참가 물질

4

반응물 2

HCID 69208Ethyl 2,4-dioxovalerateHCID 521874O-Methylhydroxylamine hydrochloride

생성물 1

HCID 589173Ethyl 2-(methoxyimino)-4-oxopentanoate수율 45.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 2.5 g of ethyl 2,4-dioxovalerate, 1.45 g of O-methylhydroxylamine hydrochloride and 10 ml of ethanol was heated to reflux for 2 hours. The reaction mixture was allowed to cool to room temperature, and partitioned between water and ethyl acetate. The organic layer was washed with water and an aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 1.34 g of ethyl 2-methoxyimino-4-oxopentanoate of the formula:

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 2 hours
  3. custompartitioned between water and ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materialan aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-5f979e7f55e24e1e8910ff9a57fb6bb4
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07867949B2

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