反应详情

温度

100 °C

To a flask charged with 3-chloroisoquinoline-7-carbonitrile (250 mg, 1.3 mmol) and a stir bar was added tert-butyl 3-oxopiperazine-1-carboxylate (400 mg, 2.0 mmol), Pd2(dba)3 (120 mg, 0.13 mmol), Xantphos (150 mg, 0.26 mmol), cesium carbonate (650 mg, 2.0 mmol), and dioxane (20 mL). The mixture was purged three times with nitrogen, and heated to 100° C. for 16 hours. The mixture was diluted with EtOAc, washed with brine, dried over sodium sulfate, adsorbed onto silica gel, and purified by silica gel chromatography (Hexanes:EtOAc) to provide tert-butyl 4-(7-cyanoisoquinolin-3-yl)-3-oxopiperazine-1-carboxylate. LC-MS (IE, m/z): 353 [M+1]+.

1. customThe mixture was purged three times with nitrogen
2. additionThe mixture was diluted with EtOAc
3. washwashed with brine
4. dry with materialdried over sodium sulfate
5. custompurified by silica gel chromatography (Hexanes:EtOAc)