Acetic Anhydride → Limonene diepoxide

HRID 1881807

반응식

HRID 1881807 반응식
[CH3:1][C:2]1[CH2:7]C[C@@H:5](C(C)=C)[CH2:4][CH:3]=1.C([O-])([O-])=[O:12].C([O-])([O-])=O.OO.OO.OO.[Na+].[Na+].[Na+].[Na+].[C:29]([O:32][C:33](=O)[CH3:34])(=O)[CH3:30]>C(OCCCC)(=O)C>[CH3:30][C:29]12[O:32][CH:33]1[CH2:34][CH:3]([C:2]1([CH3:1])[O:12][CH2:7]1)[CH2:4][CH2:5]2

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 159762Sodium percarbonateHCID 440917(+)-Limonene

생성물 1

HCID 232703Limonene diepoxide수율 99%

시약·촉매·용매 1

HCID 31272Butyl Acetate용매

반응 조건

온도
60 °C

실험 절차

Limonene (1.36 g, 10 mmol) was dissolved in butyl acetate (25 ml), and a composition containing sodium percarbonate (10.5 g, 66.7 mmol) and acetic anhydride (10.2 g, 100 mmol) was added thereto. The mixture was stirred at 60° C. After 12 hours, the reaction solution was washed with water to thereby completely remove acetic acid and sodium acetate, which were generated as by-products, and the remaining H2O2. Butyl acetate was distilled off from the organic phase by distillation, and as a result, 1.66 g (99% yields) of limonene diepoxide with a GC purity of 100% was obtained.

후처리

  1. additionwas added
  2. washthe reaction solution was washed with water to thereby completely remove acetic acid and sodium acetate, which
  3. distillationButyl acetate was distilled off from the organic phase by distillation

출처 및 근거

ORD 기록
ord-756f02b83b414ff8a3f468c19c9d140b
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08318958B2

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