HRID553902

反应详情

EQUATION

反应方程式

HRID 553902 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

IPEA (0.03 mL), HOBT (10 mg), and EDC (14 mg) were sequentially added to a solution of (E)-4-{(4S*,9aR*)-7-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)benzylidene]-6-oxooctahydroquinolizin-4-yl}benzoic acid (22 mg) and dimethylamine (2 M solution in THF, 0.12 mL) in DMF (2 mL), and the reaction solution was stirred at room temperature for two hours. Then, the reaction solution was further stirred at 100° C. for six hours. The reaction solution was left to cool to room temperature. Ethyl acetate and saturated sodium bicarbonate water were added to the reaction solution, and the organic layer was separated. The resulting organic layer was dried over magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (carrier: Chromatorex NH; elution solvent: ethyl acetate:methanol=9:1) to obtain 19 mg of the title compound. The property values of the compound are as follows.

WORKUP

后处理

  1. stirringThen, the reaction solution was further stirred at 100° C. for six hours
  2. waitThe reaction solution was left
  3. temperatureto cool to room temperature
  4. customthe organic layer was separated
  5. dry with materialThe resulting organic layer was dried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (carrier: Chromatorex NH; elution solvent: ethyl acetate:methanol=9:1)