HRID410219
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
- 170 °C
PROCEDURE
实验过程
A mixture of 4-(3-bromopyridin-2-yloxy)aniline (1.73 g, 6.53 mmol) and 2-chlorobenzoxazole (1.00 g, 6.51 mmol, TCI America) in NMP (3 mL) was sealed in a screw-cap flask and heated at 170° C. for 20 h. The reaction was cooled to rt and partitioned with water/EtOAc. The aqueous layer was extracted with EtOAc (3×) and the combined organic layers were evaporated onto silica gel and purified by flash chromatography (Isco (80 gram)) eluting with EtOAc:hexanes (0:1→1:2) a tan amorphous solid. MS (ESI, pos. ion) m/z: 382.0, 383.9 (M+1).
WORKUP
后处理
- customwas sealed in a screw-cap flask
- temperatureThe reaction was cooled to rt
- custompartitioned with water/EtOAc
- extractionThe aqueous layer was extracted with EtOAc (3×)
- customthe combined organic layers were evaporated onto silica gel
- custompurified by flash chromatography (Isco (80 gram))
- washeluting with EtOAc:hexanes (0:1→1:2) a tan amorphous solid