反应 #595356

反应方程式

compound

2-Amino-4-[4-(2-hydroxyethoxy)phenyl]-6-(phenylsulfanyl)pyridine-3,5-dicarbonitrile

sodium hydroxide

→

6-Amino-4-[4-(2-hydroxyethoxy)phenyl]-2-oxo-1,2-dihydropyridine-3,5-dicarbonitrile

溶剂

ethanol

反应条件

后处理

1. 1
   其他a clear solution is formed
2. 2
   温度After cooling to RT
3. 3
   其他the solvent is removed on a rotary evaporator
4. 4
   其他is formed
5. 5
   workup.STIRRINGThe suspension is stirred at RT for 3 h
6. 6
   过滤The precipitate is filtered off
7. 7
   洗涤washed with about 5 ml of water
8. 8
   其他a little ethanol and then recrystallized from about 10 ml of ethanol
9. 9
   其他The product obtained in this manner
10. 10
    其他is used without further purification in the subsequent reactions

实验过程

500 mg (1.29 mmol) of the compound from Example 99A are initially charged in 6.4 ml of ethanol. After addition of 2.57 g (28.96 mmol) of sodium hydroxide, the mixture is stirred at 80° C. for 30 min, and a clear solution is formed. After cooling to RT, the solvent is removed on a rotary evaporator. The residue is taken up in 3 ml of water and acidified with 1 N hydrochloric acid until a yellowish precipitate is formed. The suspension is stirred at RT for 3 h. The precipitate is filtered off, washed with about 5 ml of water and a little ethanol and then recrystallized from about 10 ml of ethanol. The product obtained in this manner is used without further purification in the subsequent reactions.

来源