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
- 80 °C
PROCEDURE
实验过程
A mixture of compound 2a (100.0 mg, 0.320 mmol), 4-(tert-butoxycarbonyl)benzeneboronic acid pinacol ester (117 mg, 0.390 mmol), dichloro(1,1′-bis(diphenylphosphino)ferrocene)palladium(II) dichloromethane adduct (24.0 mg, 0.0320 mmol), and 1M sodium carbonate (1.61 mL, 1.61 mmol) in dioxane (6 mL) was purged with Argon gas. The resulting mixture was heated to 80° C. for 18 h. After the mixture was cooled, it was filtered through a pad of diatomaceous earth. The filtrate was concentrated under reduced pressure and the resulting residue was purified by Preparative TLC (EtOAc/CH2Cl2; 2:3, v/v) to give compound 81a. Mass Spectrum (LCMS, ESI pos.): Calcd. for C22H25N4O4: 409.2 (M+H). found: 409.3.
WORKUP
后处理
- customwas purged with Argon gas
- temperatureAfter the mixture was cooled
- filtrationit was filtered through a pad of diatomaceous earth
- concentrationThe filtrate was concentrated under reduced pressure
- customthe resulting residue was purified by Preparative TLC (EtOAc/CH2Cl2