Acetic Anhydride → Limonene diepoxide

HRID 1881809

反応式

HRID 1881809 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 232703Limonene diepoxide収率 97%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
60 °C

実験手順

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.

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. distillationToluene was distilled off from the organic phase by distillation

出典と根拠

ORDレコード
ord-00efc152fb354a6f9f53c092d9d2df38
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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