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Phthalic Anhydride → 2-(5-Methylpyridin-2-yl)isoindoline-1,3-dione

HRID 1505051
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인쇄 미리보기

반응식

HRID 1505051 반응식
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([NH2:8])=[N:6][CH:7]=1.[C:9]1(=O)[O:14][C:12](=[O:13])[C:11]2=[CH:15][CH:16]=[CH:17][CH:18]=[C:10]12.CCN(C(C)C)C(C)C>C1(C)C=CC=CC=1>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[C:12](=[O:13])[C:11]3[C:10](=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:9]2=[O:14])=[N:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6811Phthalic AnhydrideHCID 153482-Amino-5-methylpyridineHCID 81531Diisopropylethylamine

생성물 1

HCID 109665522-(5-Methylpyridin-2-yl)isoindoline-1,3-dione

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture containing 5-methylpyridin-2-amine (5.4 g, 50 mmol), phthalic anhydride (8.88 g, 60 mmol) and DIEA (19 ml, 110 mmol) in toluene (30 ml) is refluxed for 18 hours, and cooled. The solvent is removed by rotary evaporation. The crude product is purified by silica gel flash chromatography to afford 2-(5-methylpyridin-2-yl)isoindoline-1,3-dione as a dark brown oil. LC-MS m/z: 239.1 (M+1).

후처리

  1. temperatureis refluxed for 18 hours
  2. temperaturecooled
  3. customThe solvent is removed by rotary evaporation
  4. customThe crude product is purified by silica gel flash chromatography

출처 및 근거

ORD 기록
ord-c767b0a952f548239499271ca6a84499
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216964B2

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