Formic Acid → 1,2-Dodecanediol

HRID 132090

반응식

HRID 132090 반응식
[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]

참가 물질

6

반응물 5

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

생성물 1

HCID 928661,2-Dodecanediol

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9dc05daf695845eabce1908a2ae43efe
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07385092B2

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