反应 #1265378

反应方程式

2,6-diamino-3-nitropyridine

phenylglyoxal hydrate

→

3-phenylpyrido[2,3-b]pyrazin-6-ylamine

溶剂

ethanol

ethanol

反应条件

后处理

1. 1
   过滤the catalyst is filtered off with suction through a glass fibre filter
2. 2
   过滤The catalyst is then filtered off under nitrogen as protective gas
3. 3
   其他The greenish blue reaction mixture
4. 4
   温度is heated
5. 5
   温度under reflux under nitrogen for 30 min
6. 6
   温度to cool
7. 7
   其他the solvent is removed in vacuo
8. 8
   其他A dark brown solid is finally obtained
9. 9
   其他Purification by column chromatography on silica gel (mobile phase dichloromethane/methanol mixture)
10. 10
    其他affords a pale yellow crystalline solid

实验过程

A solution of 1.22 g of 2,6-diamino-3-nitropyridine (7.92 mmol) in 210 ml of ethanol is hydrogenated with Raney nickel as catalyst at 50° C. and 5 bar. After the hydrogenation is complete, the catalyst is filtered off with suction through a glass fibre filter. Before the filtration, 1.68 g of phenylglyoxal hydrate (11.03 mmol) are introduced into 50 ml of ethanol in the receiver. The catalyst is then filtered off under nitrogen as protective gas, and the hydrogenation solution is sucked directly into the reaction flask. The greenish blue reaction mixture is heated under reflux under nitrogen for 30 min. The mixture is allowed to cool, and the solvent is removed in vacuo. A dark brown solid is finally obtained. Purification by column chromatography on silica gel (mobile phase dichloromethane/methanol mixture) affords a pale yellow crystalline solid.

来源