Hydrogen Peroxide → Di(1-methyl-cyclohexyl)peroxide

HRID 241467

反应方程式

HRID 241467 反应方程式
[CH3:1][C:2]1(O)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.[OH:9][OH:10]>>[CH3:1][C:2]1([O:9][O:10][C:2]2([CH3:1])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1

参与物

3

反应物 2

HCID 784Hydrogen PeroxideHCID 115501-甲基环己醇

产物 1

HCID 19090310Di(1-methyl-cyclohexyl)peroxide

实验过程

1-methylcyclohexanol (30 g, 0.26 mol) was placed in a 100 mL three necked round bottomed flask and was stirred. The flask was cooled in a brine/ice bath, dropping funnel fitted and fitted with a static N2 supply. The dropping funnel was charged with 98% sulfuric acid (16.14 ml) and water (6.45 ml) giving a 70% sulfuric acid solution. This was added dropwise to the 1-methylcyclohexanol and stirring continued to give a viscous brown mixture. The bath was recharged with ice/brine, dropping funnel rinsed with water and recharged with 35% hydrogen peroxide (6.98 mL, 0.125 mol) and added dropwise. The solution separated into two phases. Cyclohexanol (150 mL) was added and the mixture was transferred to a separating funnel. The aqueous fraction was extracted with another portion of cyclohexane (150 ml) and the combined organic fractions washed with 1M NaOH (2×100 mL), water (2×150 mL), dried and evaporated to give a viscous colourless oil. (12.98 g). The oil was sorbed onto silica gel then placed on a silica gel column and eluted with cyclohexane. After evaporation at reduced pressure 0.7 g colourless oil of di(1-methyl-cyclohexyl)peroxide was obtained. 13C-NMR (CDCl3) δ 22.45, 25.01, 25.95, 35.39, 78.58

后处理

  1. customto give a viscous brown mixture
  2. washrinsed with water
  3. additionadded dropwise
  4. customThe solution separated into two phases
  5. additionCyclohexanol (150 mL) was added
  6. customthe mixture was transferred to a separating funnel
  7. extractionThe aqueous fraction was extracted with another portion of cyclohexane (150 ml)
  8. washthe combined organic fractions washed with 1M NaOH (2×100 mL), water (2×150 mL)
  9. customdried
  10. customevaporated
  11. customto give a viscous colourless oil
  12. washeluted with cyclohexane
  13. customAfter evaporation at reduced pressure 0.7 g colourless oil of di(1-methyl-cyclohexyl)peroxide
  14. customwas obtained

来源与证据

ORD记录
ord-d3d73e14267a4536a47a06f4d4aee3b9
来源数据集
uspto-grants-2014_02
专利号
US08650742B2

关联笔记

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