HRID1096931

反应详情

EQUATION

反应方程式

HRID 1096931 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

Tert-Butyl 6-bromo-4-oxospiro[chroman-2,4′-piperidine]-1′-carboxylate (16.3 g), 5-amino-1-methyl-1H-pyrazole (4.00 g), palladium acetate (922 mg), 2-(di-t-butylphosphino)biphenyl (1.23 g) and cesium carbonate (16.1 g) were suspended in 1,4-dioxane (20 mL), and heated under reflux at 110° C. for 5 hours. The reaction liquid was filtered through Celite, the residue on the Celite was washed with chloroform, and the filtrate was concentrated under reduced pressure. The resulting residue was purified through silica gel column chromatography (hexane/EtOAc) to obtain the intended compound as a yellow amorphous solid.

WORKUP

后处理

  1. temperatureheated
  2. customThe reaction liquid
  3. filtrationwas filtered through Celite
  4. washthe residue on the Celite was washed with chloroform
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe resulting residue was purified through silica gel column chromatography (hexane/EtOAc)