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
To 10-20 mL microwave flask was added ethyl 2-(4-(7-(bis((2-(trimethylsilyl)ethoxy)methyl)amino)-3-(6-chloropyridin-3-yl)pyrazolo[1,5-a]pyrimidin-5-yl)cyclohexyl)acetate (Int-5m, 500 mg, 741 μmol), phenylboronic acid (181 mg, 1.48 mmol), K3PO4 (314 mg, 1.48 mmol), Pd(PPh3)4 (86 mg, 74 mol) and 3:1 1,4-dioxane:H2O (8 mL). The flask was flushed with argon and sealed. The reaction was stirred in a microwave at 150° C. for 30 minutes. After 30 minutes, the reaction was diluted with DCM and washed with H2O. The aqueous was extracted with DCM (x2) and the combined organic layers were dried over Na2SO4. The solvent was reduced in vacuo and the title compound was purified via silica gel chromatography.
WORKUP
后处理
- customThe flask was flushed with argon
- customsealed
- waitAfter 30 minutes
- additionthe reaction was diluted with DCM
- washwashed with H2O
- extractionThe aqueous was extracted with DCM (x2)
- dry with materialthe combined organic layers were dried over Na2SO4
- customthe title compound was purified via silica gel chromatography