Ammonia → Methyl 4-ethoxycarbonyl-3-oxopentanoate

HRID 654998노트

반응식

HRID 654998 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 14348549Methyl 4-ethoxycarbonyl-3-oxopentanoate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ff3b43f7b9cc4362acc0fed0dd6022c9
출처 데이터셋
uspto-grants-1992_07
특허 번호
US05134231

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