HRID874608
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
- 85 °C
PROCEDURE
实验过程
A mixture of 6-bromo-5-chloro-2-methylbenzoxazole (35) (123 mg, 0.5 mmol), 2-aminopyridine-5-boronic acid pinacol ester (11) (130 mg, 0.6 mmol), Bis(dicyclohexyl(4-dimethylaminophenyl)phosphine)dichloropalladium (II) (35 mg) and K3PO4 (106 mg, 0.5 mmol) in 1 ml ACN, 1 ml dioxane, 0.25 ml H2O was bubbled with argon before heated at 85° C. for 6 h. After cooling down to r.t., the reaction mixture was taken up in EA, washed with aq. NaHCO3 and brine, dried over Na2SO4, concentrated to dryness. The resulting red solid was dissolved in DCM and subjected to silica gel column purification using 0-100% B (A: hexane; B: EA) to furnish 78 mg 36 as off-white solid (yield: 60%)
WORKUP
后处理
- customwas bubbled with argon
- temperatureAfter cooling down to r.t.
- washwashed with aq. NaHCO3 and brine
- dry with materialdried over Na2SO4
- concentrationconcentrated to dryness
- dissolutionThe resulting red solid was dissolved in DCM
- customsubjected to silica gel column purification