HRID1708144
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
4.9 g (25 mmol) of 6-butyl-2-oxo-1,2-dihydro-isonicotinic acid are boiled under reflux (237° C.) for 1.5 h with 1.79 g (12.5 mmol) of copper (I) oxide in 50 ml of quinoline. 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
- filtrationAfter filtering off
- customthe volatile constituents are removed by distillation in vacuo (110° C. at 17 mbar
- custom67° C.
- customThe residue is chromatographed twice on silica gel