1,1'-Carbonyldiimidazole → 2-Oxo-2,3-dihydro-1,3-benzoxazole-5-carbonitrile
반응식
[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]1참가 물질
5
실험 절차
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.
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-5cd956fca9f84e4dbd755ecf4a20ee01
- 출처 데이터셋
- uspto-grants-2011_05
- 특허 번호
- US07951825B2
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