Methanol → HCID 22298443、化合物

HRID 1173764ノート

反応式

HRID 1173764 の反応式
[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]

参加物

5

反応物 3

HCID 887MethanolHCID 11424094Ethyl 2-chloro-3-oxohexanoateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 22298443HCID 22298443、化合物収率 72.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-8f2a9aadef7a4c1b971c7dc56892c4ea
出典データセット
uspto-grants-2010_11
特許番号
US07834190B2

反応ノート

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