Sodium Methoxide → HCID 12916445、化合物

HRID 582895ノート

反応式

HRID 582895 の反応式
Cl[CH:2]([C@H:7]([OH:10])[CH2:8][CH3:9])[C:3]([O:5][CH3:6])=[O:4].C[O-].[Na+]>CO>[O:10]1[C@H:7]([CH2:8][CH3:9])[C@H:2]1[C:3]([O:5][CH3:6])=[O:4]

参加物

4

反応物 2

HCID 10942334Sodium MethoxideHCID 54420244HCID 54420244、化合物3 回

生成物 1

HCID 12916445HCID 12916445、化合物収率 82.87%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒3 回

実験手順

To 130 ml of a methanol solution of 25.5 g (0.153 mol) of the methyl (3R)-2-chloro-3-hydroxypentanoate obtained in (2) above was added dropwise 30 g (0.155 mol) of a 28% methanol solution of sodium methoxide at 0 to 5° C., followed by stirring at room temperature for 1 hour. After confirming disappearance of the methyl (3R)-2-chloro-3-hydroxypentanoate by TLC, methanol was evaporated. The concentrate was cooled, adjusted to pH 8 to 9 with 120 ml of a phosphate buffer, and extracted with 300 ml of isopropyl ether. The isopropyl ether was evaporated, and the residue was purified by column chromatography to give 16.5 g (0.126 mol; yield: 82.87%) of the title compound.

後処理

  1. customwas evaporated
  2. temperatureThe concentrate was cooled
  3. extractionextracted with 300 ml of isopropyl ether
  4. customThe isopropyl ether was evaporated
  5. customthe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-5f6971093e0d4e9889f0a5e8d3f9f2e1
出典データセット
uspto-grants-1999_07
特許番号
US05925792

反応ノート

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