Safrole → Safrole oxide

HRID 1270644

반응식

HRID 1270644 반응식
[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

참가 물질

4

반응물 2

HCID 5144SafroleHCID 70297m-Chloroperbenzoic acid

생성물 1

HCID 101123Safrole oxide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c03c854e78a447c992e058552ddbc863
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07202261B2

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