HRID875111
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 65 °C
PROCEDURE
实验过程
A suspension of 0.20 g (0.63 mmol) of ethyl 8-[(aminocarbonyl)amino]-1-methyl-1H-pyrazolo[4,3-h]quinazoline-3-carboxylate in 15 mL of a mixture methanol/dimethylformamide/ammonium hydroxide 30% 1/1/1 was stirred in a close bottle at 65° C. for 48 hours. The solvent was then evaporated under reduced pressure, the residue redissolved with a mixture dichloromethane/methanol 9/1 and washed with water. The organic layer was dried over anhydrous Na2SO4 and evaporated to dryness. The product was purified by chromatography on a silica gel column (eluant dichloromethane/acetone/methanol) giving 0.09 g (50% yield) of the title compound.
WORKUP
后处理
- customThe solvent was then evaporated under reduced pressure
- dissolutionthe residue redissolved with a mixture dichloromethane/methanol 9/1
- washwashed with water
- dry with materialThe organic layer was dried over anhydrous Na2SO4
- customevaporated to dryness
- customThe product was purified by chromatography on a silica gel column (eluant dichloromethane/acetone/methanol)