Safrole → Safrole oxide

HRID 1060378

反応式

HRID 1060378 の反応式
[O:1]1[C:12]2[C:4](=[CH:5][C:6](=[CH:10][CH:11]=2)[CH2:7][CH:8]=[CH2:9])[O:3][CH2:2]1.ClC1C=C(C=CC=1)C(OO)=[O:18]>C(Cl)Cl>[O:1]1[C:12]2[C:4](=[CH:5][C:6](=[CH:10][CH:11]=2)[CH2:7][CH:8]2[O:18][CH2:9]2)[O:3][CH2:2]1

参加物

4

反応物 2

HCID 5144SafroleHCID 70297m-Chloroperbenzoic acid

生成物 1

HCID 101123Safrole oxide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Safrole oxide was prepared by stirring a solution of safrole (1.48 mL, 10 mmol) and m-chloroperoxybenzoic acid (2.70 g, 11 mmol) in methylene dichloride (25 mL) overnight. The reaction was quenched by pouring into water (50 mL). The aqueous was extracted with ether (3×25 mL). The organic layers were combined and washed with 10% aqueous sodium sulfate (2×25 mL), saturated aqueous sodium bicarbonate (3×25 mL), and brine (25 mL). The organic phase was dried over magnesium sulfate and the solvents were removed in vacuo. The resulting yellow oil was used without further purification.

後処理

  1. customThe reaction was quenched
  2. additionby pouring into water (50 mL)
  3. extractionThe aqueous was extracted with ether (3×25 mL)
  4. washwashed with 10% aqueous sodium sulfate (2×25 mL), saturated aqueous sodium bicarbonate (3×25 mL), and brine (25 mL)
  5. dry with materialThe organic phase was dried over magnesium sulfate
  6. customthe solvents were removed in vacuo
  7. customThe resulting yellow oil was used without further purification

出典と根拠

ORDレコード
ord-a19d73b883a4457abb2e2e5915d4eb80
出典データセット
uspto-grants-2003_02
特許番号
US06521667B1

関連ノート

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