Safrole → Safrole oxide

HRID 1060378Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1060378
[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

Komponenten

4

Edukt 2

HCID 5144SafroleHCID 70297m-Chloroperbenzoic acid

Produkt 1

HCID 101123Safrole oxide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-a19d73b883a4457abb2e2e5915d4eb80
Quelldatensatz
uspto-grants-2003_02
Patentnummer
US06521667B1

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