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
- 150 °C
PROCEDURE
实验过程
200 mg (0.44 mmol, purity 85%) of the compound from Example 2A and 199 mg (0.57 mmol) of the compound of Example 46A in 2.18 ml of 1,4-dioxane were degassed with argon. 9.9 mg (0.044 mmol) of palladium(II) acetate, 38.3 mg (0.066 mmol) of xantphos and 431 mg (1.32 mmol) of caesium carbonate were added and the mixture was heated in a microwave oven (Biotage Initiator, with Dynamic Field Tuning) at 150° C. for 30 min. The reaction was then filtered through kieselguhr and the filtrate was concentrated. The residue was subjected to flash-chromatography on silica gel (mobile phase dichloromethane/ethyl acetate 1:1). The product fractions were concentrated under reduced pressure and the residue was dried. This gave 180 mg (63% of theory) of the title compound.
WORKUP
后处理
- filtrationThe reaction was then filtered through kieselguhr
- concentrationthe filtrate was concentrated
- concentrationThe product fractions were concentrated under reduced pressure
- customthe residue was dried