Acetic Anhydride → Limonene diepoxide

HRID 1881811

반응식

HRID 1881811 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 97%

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 (6.0 g, 38.1 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, 1.63 g (97% yields) of limonene diepoxide with a GC purity of 97% were 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-ee42dbb0025f4eb69d6c6a9cc16241ea
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08318958B2

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