Ammonia → Methyl 4-ethoxycarbonyl-3-oxopentanoate

HRID 654998ノート

反応式

HRID 654998 の反応式
[O:1]=[C:2]([CH:10]([C:14]([O:16][CH3:17])=[O:15])C(=O)C)[CH:3]([CH3:9])[C:4]([O:6][CH2:7][CH3:8])=[O:5].N>O1CCCC1>[CH2:7]([O:6][C:4]([CH:3]([CH3:9])[C:2](=[O:1])[CH2:10][C:14]([O:16][CH3:17])=[O:15])=[O:5])[CH3:8]

参加物

4

反応物 2

HCID 222AmmoniaHCID 14348548Ethyl 3,5-dioxo-4-methoxycarbonyl-2-methylhexanoate

生成物 1

HCID 14348549Methyl 4-ethoxycarbonyl-3-oxopentanoate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Ethyl 3,5-dioxo-4-methoxycarbonyl-2-methylhexanoate (176 mg; 0.72 mmole) was dissolved in tetrahydrofuran (1.3 ml), and 1.7N aqueous ammonia (0.85 ml) was added thereto at room temperature. The resultant mixture was allowed to stand at the same temperature overnight, followed by removal of tetrahydrofuran under reduced pressure. The reaction mixture was combined with lN hydrochloric acid (0.7 ml) and an aqueous sodium chloride solution and extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give methyl 4-ethoxycarbonyl-3-oxopentanoate.

後処理

  1. customat room temperature
  2. customto stand at the same temperature overnight
  3. customfollowed by removal of tetrahydrofuran under reduced pressure
  4. extractionan aqueous sodium chloride solution and extracted with ethyl acetate
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate and anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-ff3b43f7b9cc4362acc0fed0dd6022c9
出典データセット
uspto-grants-1992_07
特許番号
US05134231

反応ノート

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