HRID1395457

反应详情

EQUATION

反应方程式

HRID 1395457 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 6.2 g. (0.03 mole) of 2,3,4,4a-tetrahydro-1H-pyrazino[1,2-a]quinoxalin-5(6H)-one, hydrochloride in 200 ml. acetone is added 15 g. of powdered potassium carbonate, 0.5 ml. of triethylamine, 5 g. of potassium iodide, and 7 g. (0.038 mole) of 5-(4-pyridyl)pentyl bromide. The suspension is stirred and refluxed for 72 hours, cooled, and filtered. The filtrate is concentrated under reduced pressure and the residue is dissolved in methylene dichloride, washed with saline, and dried. The dried organic layer is concentrated and the residue purified by column chromatography using Silicar CC-7. This title compound is obtained as base and converted to hydrochloride salt.

WORKUP

后处理

  1. temperaturerefluxed for 72 hours
  2. temperaturecooled
  3. filtrationfiltered
  4. concentrationThe filtrate is concentrated under reduced pressure
  5. dissolutionthe residue is dissolved in methylene dichloride
  6. washwashed with saline
  7. customdried
  8. concentrationThe dried organic layer is concentrated
  9. customthe residue purified by column chromatography