Acetic Anhydride → Limonene diepoxide

HRID 1881811

反応式

HRID 1881811 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 232703Limonene diepoxide収率 97%

試薬・触媒・溶媒 1

HCID 31272Butyl Acetate溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ee42dbb0025f4eb69d6c6a9cc16241ea
出典データセット
uspto-grants-2012_11
特許番号
US08318958B2

関連ノート

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