HRID838850
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
5,7-Dimethyl pyrazolo[1,5-a]pyrimidine [1.0g (6.8 mmoles)] was dissolved in H2SO4 (10 ml) keeping the temperature below 5°. Fuming HNO3 [4 ml; sp. gr. 1.5] was added dropwise to the cold H2SO4 solution, with good stirring. The temperature during this addition was maintained below 10°. After the addition was complete, the solution was stirred at room temperature for 45 minutes and then added to 100 g of ice. The precipitated product was separated by filtration, washed well with H2O, and dried. Recrystallization from CH3OH afforded 0.75 g (57%) of analytically pure product; mp 156°-7°.
WORKUP
后处理
- customthe temperature below 5°
- additionThe temperature during this addition
- temperaturewas maintained below 10°
- additionAfter the addition
- customThe precipitated product was separated by filtration
- washwashed well with H2O
- customdried
- customRecrystallization from CH3OH
- customafforded 0.75 g (57%) of analytically pure product