반응 #72871

반응 방정식

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

수율 85.0%

용매

sodium ethylate

ethanol

반응 조건

후처리

1. 1
   온도at reflux for 12 hours
2. 2
   기타The solvent was then evaporated
3. 3
   workup.DISSOLUTIONthe residue redissolved with dichloromethane
4. 4
   세척washed with water
5. 5
   건조The organic layer was then dried over anhydrous Na2SO4
6. 6
   농축concentrated
7. 7
   기타The residue was triturated with diethyl ether
8. 8
   여과the product collected by filtration (85% yield as a white solid)

실험 절차

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).

출처