تفاعل #595356
ord-963d645643a140edb98468049189ceca
معادلة التفاعل
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
المتفاعلات
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىa clear solution is formed
- 2درجة الحرارةAfter cooling to RT
- 3أخرىthe solvent is removed on a rotary evaporator
- 4أخرىis formed
- 5workup.STIRRINGThe suspension is stirred at RT for 3 h
- 6ترشيحThe precipitate is filtered off
- 7غسيلwashed with about 5 ml of water
- 8أخرىa little ethanol and then recrystallized from about 10 ml of ethanol
- 9أخرىThe product obtained in this manner
- 10أخرىis used without further purification in the subsequent reactions
الإجراء التجريبي
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.