反应 #72871

反应方程式

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

收率 85.0%

溶剂

sodium ethylate

ethanol

反应条件

后处理

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

实验过程

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).

来源