HRID1267117

反应详情

EQUATION

反应方程式

HRID 1267117 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 4-(4-bromo-phenyl)-3,6-dihydro-2H-pyridine-1-carboxylic acid tert-butyl ester (0.34 g), benzylamine (0.12 g) and sodium tert-butoxide (0.13 g) in toluene (8 mL) were added tris(dibenzylidene acetone)dipalladium (2.2 mg) and Binap (4.6 mg) and the mixture was heated at 80° C. for 16 hours. The solution was then cooled to room temperature, filtered and the filtrate was evaporated under reduced pressure. The residue was purified by flash chromatography eluting with petroleum ether/AcOEt (90/10) and the oily residue was crystallized from diisopropyl ether to give the title compound (0.27 g) as white crystals.

WORKUP

后处理

  1. temperatureThe solution was then cooled to room temperature
  2. filtrationfiltered
  3. customthe filtrate was evaporated under reduced pressure
  4. customThe residue was purified by flash chromatography
  5. washeluting with petroleum ether/AcOEt (90/10)
  6. customthe oily residue was crystallized from diisopropyl ether