Phthalic Anhydride → 2-(5-Methylpyridin-2-yl)isoindoline-1,3-dione
反応式
[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]=1参加物
5
実験手順
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).
後処理
- temperatureis refluxed for 18 hours
- temperaturecooled
- customThe solvent is removed by rotary evaporation
- customThe crude product is purified by silica gel flash chromatography
出典と根拠
- ORDレコード
- ord-c767b0a952f548239499271ca6a84499
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09216964B2
反応ノート
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