HRID2085942

反应详情

EQUATION

反应方程式

HRID 2085942 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

6-Chloro-pyrido[3,4-d]pyrimidin-4one (10 g) in 1-methyl-2-pyrrolidinone (100 ml) was treated with copper (I) iodide (10.52 g) and potassium cyanide (7.10 g) at 215° C. for 72 hours under N2. Further potassium cyanide was added (3.58 g) and heating continued at 230° C. for 70 hours. The 1-methyl-2-pyrrolidinone was removed by distillation at reduced pressure and the residue absorbed onto silica. Chromatography gave the title compound (2.4 g) as a beige solid; δH [2H6]DMSO 13.0(1H,bs), 9.25 (1H,s), 8.55 (1H,s), 8.50 (1H,s); m/z (M-1+) 171.

WORKUP

后处理

  1. temperatureheating
  2. customThe 1-methyl-2-pyrrolidinone was removed by distillation at reduced pressure
  3. customthe residue absorbed onto silica