1,1'-Carbonyldiimidazole → 2-Oxo-2,3-dihydro-1,3-benzoxazole-5-carbonitrile
反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[OH:10])[C:5]#[N:6].C1N=CN([C:16](N2C=NC=C2)=[O:17])C=1>CN(C=O)C.O>[O:17]=[C:16]1[NH:1][C:2]2[CH:3]=[C:4]([C:5]#[N:6])[CH:7]=[CH:8][C:9]=2[O:10]1参加物
5
実験手順
To a solution of 3-amino-4-hydroxybenzonitrile (730 mg) in DMF (10 ml) was added CDI (1.06 g) at 0° C., followed by stirring at room temperature for 3.5 hours. The reaction solution was diluted with water (10 ml), and extracted with EtOAc (200 ml). The organic layer was dried over anhydrous MgSO4, and then filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:CH3OH=98:2 to 93:7) to obtain 2-oxo-2,3-dihydro-1,3-benzoxazole-5-carbonitrile (647 mg) as a pale yellow solid.
後処理
- extractionextracted with EtOAc (200 ml)
- dry with materialThe organic layer was dried over anhydrous MgSO4
- filtrationfiltered
- concentrationthe filtrate was concentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (chloroform:CH3OH=98:2 to 93:7)
出典と根拠
- ORDレコード
- ord-5cd956fca9f84e4dbd755ecf4a20ee01
- 出典データセット
- uspto-grants-2011_05
- 特許番号
- US07951825B2
反応ノート
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