تفاعل #72871

معادلة التفاعل

guanidine hydrochloride

ethyl-6-[(dimethylamino)methylene]-1-methyl-7-oxo-4,5,6,7-tetrahydro-1H-indazole-3-carboxylate

→

Ethyl 8-amino-1-methyl-1H-pyrazolo[4,3-h]quinazoline-3-carboxylate

المردود 85.0%

المذيبات

sodium ethylate

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةat reflux for 12 hours
2. 2
   أخرىThe solvent was then evaporated
3. 3
   workup.DISSOLUTIONthe residue redissolved with dichloromethane
4. 4
   غسيلwashed with water
5. 5
   تجفيفThe organic layer was then dried over anhydrous Na2SO4
6. 6
   تركيزconcentrated
7. 7
   أخرىThe residue was triturated with diethyl ether
8. 8
   ترشيحthe product collected by filtration (85% yield as a white solid)

الإجراء التجريبي

16.00 g (0.06 mol) of ethyl-6-[(dimethylamino)methylene]-1-methyl-7-oxo-4,5,6,7-tetrahydro-1H-indazole-3-carboxylate were dissolved in 600 mL of ethanol and 3.90 g of sodium ethylate, and 5.44 g of guanidine hydrochloride were added consecutively. The solution was stirred at reflux for 12 hours. The solvent was then evaporated, the residue redissolved with dichloromethane and washed with water. The organic layer was then dried over anhydrous Na2SO4 and concentrated. The residue was triturated with diethyl ether and the product collected by filtration (85% yield as a white solid).

المصدر