HRID249841
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
- 90 °C
PROCEDURE
实验过程
A mixture of methyl 2-chlorobenzoxazole-4-carboxylate (350 mg, 1.65 mmol), 4-aminopyridine (233 mg, 2.48 mmol), palladium(II) acetate (7.4 mg, 0.033 mmol), 2-dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl (39 mg, 0.083 mmol), K2CO3 (570 mg, 4.13 mmol) and t-BuOH (4 mL) was heated to 90° C. for 40 min. After cooling to room temperature, the reaction mixture was filtered through diatomaceous earth and concentrated. The crude product was purified by column chromatography (silica gel, 9:1 CH2Cl2/CH3OH) to afford methyl 2-(pyridin-4-ylamino)benzoxazole-4-carboxylate. 1H NMR and MS consistent.
WORKUP
后处理
- temperatureAfter cooling to room temperature
- filtrationthe reaction mixture was filtered through diatomaceous earth
- concentrationconcentrated
- customThe crude product was purified by column chromatography (silica gel, 9:1 CH2Cl2/CH3OH)