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

HRID 251947

反応式

HRID 251947 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 589173Ethyl 2-(methoxyimino)-4-oxopentanoate収率 45.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-5f979e7f55e24e1e8910ff9a57fb6bb4
出典データセット
uspto-grants-2011_01
特許番号
US07867949B2

関連ノート

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