HRID1656319

反应详情

EQUATION

反应方程式

HRID 1656319 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4.9 g (25 mmol) of 6-butyl-2-oxo-1,2-dihydro-isonicotinic acid are refluxed for 1.5 h with 1.79 g (12.5 mmol) of copper(I) oxide in 50 ml of quinoline (237° C). After filtering off, the volatile constituents are removed by distillation in vacuo (110° C. at 17 mbar, then 67° C. at 9 mbar). The residue is chromatographed twice on silica gel using dichloromethane/methanol (40:1) → (20:1) and the product is stirred in petroleum ether.

WORKUP

后处理

  1. filtrationAfter filtering off
  2. customthe volatile constituents are removed by distillation in vacuo (110° C. at 17 mbar
  3. custom67° C.
  4. customThe residue is chromatographed twice on silica gel