HRID2080304
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 125 °C
PROCEDURE
实验过程
A mixture of benzyl 4-((R)-2-((6-chloro-2-(2-(tetrahydro-2H-pyran-2-yl)ethylamino)nicotinamido)methyl)pyrrolidin-1-yl)-4-oxobutylcarbamate (62 mg, 0.101 mmol), 2-cyanophenyl boronic acid (23 mg, 0.156 mmol), PdCl2(dppf)2 (11 mg, 0.02 mmol), K2CO3(92 g, 0.667 mmol) and anhydrous DMF (1 mL) was stirred at 125° C. for 1 hr. The mixture was filtered through the silica gel pad and washed with EtOAc. The filtrate was concentrated to dryness and purified on RP-HPLC using a mixture of acetonitrile and H2O to give benzyl 4-((R)-2-((6-(2-cyanophenyl)-2-(2-(tetrahydro-2H-pyran-2-yl)ethylamino)nicotinamido)methyl)pyrrolidin-1-yl)-4-oxobutylcarbamate (50 mg, 77%). LRMS (M+H+) m/z 653.3.
WORKUP
后处理
- filtrationThe mixture was filtered through the silica gel pad
- washwashed with EtOAc
- concentrationThe filtrate was concentrated to dryness
- custompurified on RP-HPLC
- additiona mixture of acetonitrile and H2O