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m-Chloroperbenzoic acid → 2-(1,3-Dioxoisoindolin-2-yl)-5-methylpyridine 1-oxide

HRID 1890740
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반응식

HRID 1890740 반응식
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[C:16](=[O:17])[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[C:9]2=[O:18])=[N:6][CH:7]=1.C1C=C(Cl)C=C(C(OO)=[O:27])C=1>C(Cl)Cl>[O:17]=[C:16]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9](=[O:18])[N:8]1[C:5]1[CH:4]=[CH:3][C:2]([CH3:1])=[CH:7][N+:6]=1[O-:27]
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참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 109665522-(5-Methylpyridin-2-yl)isoindoline-1,3-dione

생성물 1

HCID 672124072-(1,3-Dioxoisoindolin-2-yl)-5-methylpyridine 1-oxide

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 2-(5-methylpyridin-2-yl)isoindoline-1,3-dione (1.62 g, 6.8 mmol) in DCM (32 ml) is added mCPBA (4.1 g, 18.2 mmol) in small portions at room temperature, and the solution is then stirred at room temperature overnight. The solution is diluted with dichloromethane, washed with aqueous Na2CO3 solution, dried over Na2SO4 and concentrated to afford 2-(1,3-dioxoisoindolin-2-yl)-5-methylpyridine 1-oxide as a brown solid. It is used without further purification in the next step. LC-MS m/z: 254.1 (M+1).

후처리

  1. washwashed with aqueous Na2CO3 solution
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-a7d156692b9c4a9f8512104e9c1175e8
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08507491B2

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