HRID1031487
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
- 100 °C
PROCEDURE
实验过程
A mixture of 2-bromo-3-methoxy pyridine (9.9 g) and (1S,4S)-N-benzyl-2,5-diazabicyclo[2.2.1]heptane (10.9 g) was heated at 100° C. in a Parr bomb for 67 h. The reaction mixture was cooled to 23° C., dissolved in CH2Cl2, extracted with 5% NaHCO3, and finally wit:h H2O. The organic layer was dried over K2CO3, filtered, and concentrated under reduced pressure. The crude oil was purified by silica gel chromatography (CH2Cl2 :MeOH; 96:4) to give the desired product (7.93 g, 51%).
WORKUP
后处理
- temperatureThe reaction mixture was cooled to 23° C.
- extractionextracted with 5% NaHCO3, and finally wit
- dry with materialThe organic layer was dried over K2CO3
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe crude oil was purified by silica gel chromatography (CH2Cl2 :MeOH; 96:4)