m-Chloroperbenzoic acid → 3-[(3-Isopropyl-oxazolidin-2-on-5-yl)methoxy]-6-methyl-pyridine-1-oxide

HRID 647979노트

반응식

HRID 647979 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH:12]([N:15]1[CH2:19][CH:18]([CH2:20][O:21][C:22]2[CH:23]=[N:24][C:25]([CH3:28])=[CH:26][CH:27]=2)[O:17][C:16]1=[O:29])([CH3:14])[CH3:13]>ClCCl>[CH:12]([N:15]1[CH2:19][CH:18]([CH2:20][O:21][C:22]2[CH:23]=[N+:24]([O-:9])[C:25]([CH3:28])=[CH:26][CH:27]=2)[O:17][C:16]1=[O:29])([CH3:14])[CH3:13]

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 204834455-{[(6-Methylpyridin-3-yl)oxy]methyl}-3-(propan-2-yl)-1,3-oxazolidin-2-one

생성물 1

HCID 204834313-[(3-Isopropyl-oxazolidin-2-on-5-yl)methoxy]-6-methyl-pyridine-1-oxide

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 4.1 g of m-chloroperbenzoic acid in 30 ml of dichloromethane is added over the course of 10 minutes to a solution of 4.8 g of 3-isopropyl-5-[(6-methylpyridin-3-yloxy)methyl]-oxazolidin-2-one in 50 ml of dichloromethane, whilst stirring, and the mixture is left to stand overnight at room temperature. After dilution with 50 ml of dichloromethane the reaction mixture is extracted with 20 ml of saturated potassium bicarbonate solution at a time, dried over sodium sulphate and evaporated in vacuo. The crystalline residue is recrystallised from dichloromethane-ether. 3-[(3-Isopropyloxazolidin-2-on-5-yl)methoxy]-6-methyl-pyridine-1-oxide, thus obtained, melts at 137°-139° C.

후처리

  1. waitthe mixture is left
  2. extractionAfter dilution with 50 ml of dichloromethane the reaction mixture is extracted with 20 ml of saturated potassium bicarbonate solution at a time
  3. dry with materialdried over sodium sulphate
  4. customevaporated in vacuo
  5. customThe crystalline residue is recrystallised from dichloromethane-ether

출처 및 근거

ORD 기록
ord-0105d3af82ca40849a74f2c7564ea8fb
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04410530

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