Methanol → HCID 22298443, 화합물

HRID 1173764노트

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HRID 1173764 반응식
[Cl:1][CH:2]([C:8](=[O:12])[CH2:9][CH2:10][CH3:11])[C:3]([O:5][CH2:6][CH3:7])=[O:4].CO.[H][H]>O>[Cl:1][CH:2]([CH:8]([OH:12])[CH2:9][CH2:10][CH3:11])[C:3]([O:5][CH2:6][CH3:7])=[O:4]

참가 물질

5

반응물 3

HCID 887MethanolHCID 11424094Ethyl 2-chloro-3-oxohexanoateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 22298443HCID 22298443, 화합물수율 72.3%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
70 °C

실험 절차

Ethyl 2-chloro-3-oxohexanoate (2.5 g, 13 mmol), methanol (7.5 ml) and water (0.75 ml) were mixed, and nitrogen substitution was carried out after reducing the pressure. The above catalyst solution was added thereto, and hydrogen substitution (3 atmospheres) was carried out under reduced pressure. The mixture was stirred at 70° C. for 14 hours. After the mixture was cooled to room temperature, the solvent was evaporated away under reduced pressure. The concentrated matter was purified by silica gel column chromatography to obtain the title compound as a colorless oil (1.83 g, yield: 72%) ((2S,3R):(2S,3S):(2R,3S):(2R,3R)=6.2:58.5:33.2:2.2).

후처리

  1. additionThe above catalyst solution was added
  2. temperatureAfter the mixture was cooled to room temperature
  3. customthe solvent was evaporated away under reduced pressure
  4. customThe concentrated matter was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-8f2a9aadef7a4c1b971c7dc56892c4ea
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07834190B2

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