HRID1031487

反应详情

EQUATION

反应方程式

HRID 1031487 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction mixture was cooled to 23° C.
  2. extractionextracted with 5% NaHCO3, and finally wit
  3. dry with materialThe organic layer was dried over K2CO3
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe crude oil was purified by silica gel chromatography (CH2Cl2 :MeOH; 96:4)