O-Methylhydroxylamine hydrochloride → HCID 53883597, 화합물

HRID 1439878노트

반응식

HRID 1439878 반응식
O=[C:2]([CH2:8][C:9](=[O:14])[CH2:10][CH2:11][CH2:12][CH3:13])[C:3]([O:5][CH2:6][CH3:7])=[O:4].Cl.[CH3:16][O:17][NH2:18]>C(O)C>[CH3:16][O:17][N:18]=[C:2]([CH2:8][C:9](=[O:14])[CH2:10][CH2:11][CH2:12][CH3:13])[C:3]([O:5][CH2:6][CH3:7])=[O:4]

참가 물질

4

반응물 2

HCID 521874O-Methylhydroxylamine hydrochlorideHCID 10998024Ethyl 2,4-dioxooctanoate

생성물 1

HCID 53883597HCID 53883597, 화합물수율 72.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To an ethanol (100 ml) solution of ethyl 2,4-dioxooctanoate (20 g) (K. Seki et al., Chem. Pharm. Bull., 32, 1568(1984)) was added, under ice-cooling, methoxyamine hydrochloride (8.4 g), and the mixture was stirred for one hour, then it was stirred for further 15 hours at room temperature. The reaction mixture was concentrated under reduced pressure, to which was added a saturated aqueous solution of sodium hydrogencarbonate, followed by extraction with ether. The extract solution was dried over anhydrous sodium sulfate, then the solvent was distilled off under reduced pressure. The residue was purified by column chromatography on silica gel to afford the title compound as a colorless oil (16.6 g, 72%).

후처리

  1. temperaturecooling
  2. concentrationThe reaction mixture was concentrated under reduced pressure, to which
  3. additionwas added a saturated aqueous solution of sodium hydrogencarbonate
  4. extractionfollowed by extraction with ether
  5. dry with materialThe extract solution was dried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-dbca3273396c410ca29bbd87004d8f6a
출처 데이터셋
uspto-grants-1996_03
특허 번호
US05496835

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