4-(4-bromo-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-5-yl)-2-chlorobenzonitrile → 5-(3-chloro-4-cyanophenyl)-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazole-4-carbonitrile
反応式
Br[C:2]1[CH:3]=[N:4][N:5]([CH:16]2[CH2:21][CH2:20][CH2:19][CH2:18][O:17]2)[C:6]=1[C:7]1[CH:14]=[CH:13][C:10]([C:11]#[N:12])=[C:9]([Cl:15])[CH:8]=1.[Cu][C:23]#[N:24]>CN(C)C=O>[Cl:15][C:9]1[CH:8]=[C:7]([C:6]2[N:5]([CH:16]3[CH2:21][CH2:20][CH2:19][CH2:18][O:17]3)[N:4]=[CH:3][C:2]=2[C:23]#[N:24])[CH:14]=[CH:13][C:10]=1[C:11]#[N:12]参加物
4
反応条件
- 温度
- 190 °C
実験手順
4-(4-bromo-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-5-yl)-2-chlorobenzonitrile (3 g, 8.18 mmol), copper(I) cyanide (0.733 g, 8.18 mmol) and N,N-dimethyl formamide (15 ml) were loaded in a microwave reactor tube. The mixture was heated 190° C. for 5 h. The reaction was quenched by pouring the mixture into 200 ml of 12% ammonia solution and stirred for 30 min. The precipitate was filtered, washed with water and dried in vacuum at 40° C. The product was used in the next step without further purification. LC-MS: [M+1]=313.75.