HRID734306
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 the solution of 3-bromo-4-chloro-furo[3,2-c]pyridine (3.0 g) in 40 ml of dioxane was added 28% ammonia solution (15 ml) in an autoclave and put into the oil bath. The reaction mixture was allowed to heat up to 150° C. and stir for 5 days at 150° C. The resultant mixture was poured into ethyl acetate and brine. The organic phases was separated, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The residue was purified by chromatography on a silica gel column to afford 3-bromo-furo[3,2-c]pyridin-4-ylamine (1.3 g). 1H NMR (400 MHz, CDCl3) ppm 7.93 (d, J=6.1 Hz, 1H), 7.52 (s, 1H), 6.87 (d, J=5.8 Hz, 1H). MS: m/z 213, 215 (M+H)+.
WORKUP
后处理
- customThe organic phases was separated
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe residue was purified by chromatography on a silica gel column