Formic Acid → 1,2-Dodecanediol

HRID 132090

反応式

HRID 132090 の反応式
[CH2:1]=[CH:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11]C.[CH:13]([OH:15])=O.OO.CO.S(=O)(=O)(O)[OH:21]>>[CH2:13]([OH:15])[CH:11]([OH:21])[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][CH3:1]

参加物

6

反応物 5

HCID 284Formic AcidHCID 784Hydrogen PeroxideHCID 887MethanolHCID 1118Sulfuric AcidHCID 81831-Dodecene

生成物 1

HCID 928661,2-Dodecanediol

反応条件

温度
100 °C

実験手順

168.3 g (1.0 mol) of 1-dodecene and 73.6 g (1.6 mol) of formic acid were mixed. This mixture was heated to 100° C. and then 115.7 g (1.7 mol) of 50% strength hydrogen peroxide solution were added dropwise over a period of 2 hours. The mixture was then stirred at 100° C. for 45 min. 64.1 g (2 mol) of methanol and 0.1 g of concentrated sulfuric acid were added, and the mixture was heated under reflux for 30 min and then the methyl formate, methanol and water were removed by distillation under atmospheric pressure. A >99% pure main fraction was isolated after the subsequent workup by distillation. The freshly distilled target product had an unpleasant, pungent odor.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 30 min
  3. customthe methyl formate, methanol and water were removed by distillation under atmospheric pressure
  4. customA >99% pure main fraction was isolated after the subsequent workup
  5. distillationby distillation

出典と根拠

ORDレコード
ord-9dc05daf695845eabce1908a2ae43efe
出典データセット
uspto-grants-2008_06
特許番号
US07385092B2

関連ノート

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