反応 #595356

反応方程式

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

溶媒

ethanol

反応条件

後処理

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

実験手順

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.

出典