m-Chloroperbenzoic acid → HCID 20030875, 화합물

HRID 232211노트

반응식

HRID 232211 반응식
[Cl:1][C:2]1([C:15]([O:17][CH:18]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[O:16])[CH:6](SC2C=CC=CC=2)[CH2:5][C:4](=[O:14])[O:3]1.ClC1C=CC=C(C(OO)=O)C=1>ClCCl>[Cl:1][C:2]1([C:15]([O:17][CH:18]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)=[O:16])[CH:6]=[CH:5][C:4](=[O:14])[O:3]1

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 57046507Diphenylmethyl 2-chloro-3-phenylthio-5-oxo-2-tetrahydrofuran carboxylate

생성물 1

HCID 20030875HCID 20030875, 화합물수율 66.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In 10 ml of dichloromethane was dissolved 0.30 g of the Compound (48) obtained in Example 48. To the solution was added 150 mg of 3-chloroperbenzoic acid. The mixture was stirred at room temperature for 30 minutes. The reaction solution was washed with an aqueous solution of sodium hydrogen carbonate and water, successively. The resultant was dried (Na2SO4), and the solvent was evaporated off. The residue was dissoved in 6 ml of toluene, and the solution was heated at 60° C. for 30 minutes, then the solvent was evaporated off. The residue was subjected to a silica gel column chromatography, followed by elution with hexane-ethyl acetate (5:1) to give 0.15 g of the subject Compound (49) as colorless crystals. Recrystallization from ethyl acetatehexane to give colorless needless, m.p. 99°-101° C.

후처리

  1. washThe reaction solution was washed with an aqueous solution of sodium hydrogen carbonate and water
  2. dry with materialThe resultant was dried (Na2SO4)
  3. customthe solvent was evaporated off
  4. temperaturethe solution was heated at 60° C. for 30 minutes
  5. customthe solvent was evaporated off
  6. washfollowed by elution with hexane-ethyl acetate (5:1)

출처 및 근거

ORD 기록
ord-a87152415f9f46b0a3060609fbd35de1
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04851422

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