Acetic Anhydride → Limonene diepoxide

HRID 1881809

반응식

HRID 1881809 반응식
[CH3:1][C:2]1[CH2:7][CH2:6][C@@H:5]([C:8]([CH3:10])=[CH2:9])[CH2:4][CH:3]=1.B1([O-])OO1.[OH2:15].[OH2:16].O.O.[Na+].C(OC(=O)C)(=O)C>C1(C)C=CC=CC=1>[CH3:1][C:2]12[O:15][CH:7]1[CH2:6][CH:5]([C:8]1([CH3:10])[O:16][CH2:9]1)[CH2:4][CH2:3]2

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 440917(+)-LimoneneHCID 23693097Sodium;3-oxidodioxaborirane;tetrahydrate

생성물 1

HCID 232703Limonene diepoxide수율 97%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
60 °C

실험 절차

Limonene (1.36 g, 10 mmol) was dissolved in toluene (25 ml), and a composition containing sodium perborate tetrahydrate (15.4 g, 100 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. Toluene 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 98% 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. distillationToluene was distilled off from the organic phase by distillation

출처 및 근거

ORD 기록
ord-00efc152fb354a6f9f53c092d9d2df38
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08318958B2

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