反応 #72871

反応方程式

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

収率 85.0%

溶媒

sodium ethylate

ethanol

反応条件

後処理

1. 1
   温度at reflux for 12 hours
2. 2
   その他The solvent was then evaporated
3. 3
   workup.DISSOLUTIONthe residue redissolved with dichloromethane
4. 4
   洗浄washed with water
5. 5
   乾燥The organic layer was then dried over anhydrous Na2SO4
6. 6
   濃縮concentrated
7. 7
   その他The residue was triturated with diethyl ether
8. 8
   ろ過the product collected by filtration (85% yield as a white solid)

実験手順

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).

出典