Dimethylformamide → 3-Chloroisoquinoline-7-carbonitrile
반응식
Br[C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[C:7]([Cl:12])[N:8]=[CH:9]2)=[CH:4][CH:3]=1.[Cu][C:14]#[N:15].CN(C=O)C>CCOC(C)=O>[Cl:12][C:7]1[N:8]=[CH:9][C:10]2[C:5]([CH:6]=1)=[CH:4][CH:3]=[C:2]([C:14]#[N:15])[CH:11]=2참가 물질
5
반응 조건
- 온도
- 150 °C
실험 절차
To a flask charged with 7-bromo-3-chloroisoquinoline (1.0 g, 4.1 mmol) and a stir bar was added copper(I) cyanide (550 mg, 6.2 mmol) and DMF (50 mL). The mixture was heated to 150° C. for 24 hours under an atmosphere of nitrogen. The reaction was diluted with EtOAc, washed with sat. NH4OAc and brine, dried over sodium sulfate, concentrated and purified by silica gel chromatography (Hexanes:DCM) and the solvent removed to afford the title compound. LC-MS (IE, m/z): 189 [M+1]+.
후처리
- washwashed with sat. NH4OAc and brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated
- custompurified by silica gel chromatography (Hexanes:DCM)
- customthe solvent removed
출처 및 근거
- ORD 기록
- ord-17efae57b70342efa32828aeef1cd4d0
- 출처 데이터셋
- uspto-grants-2015_04
- 특허 번호
- US08999991B2
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