HRID570530
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
615 mg (3.27 mmol) of dimethyl 2,2-dimethyl-3-oxobutanedioate were initially charged in 13 ml of ethanol and heated to reflux. Subsequently, 652 mg (2.18 mmol) of 1-(2-fluorobenzyl)-6-methyl-1H-pyrazolo[3,4-d]pyrimidine-3-carboximidohydrazide suspended in 13 ml of ethanol were added and the mixture was boiled under reflux overnight. After cooling, the mixture was filtered, the filtercake was washed with a little ethanol and the filtrate was concentrated. The residue was purified by means of preparative HPLC (eluent: acetonitrile/water, gradient 30:70→100:0). 182 mg of the target compound were obtained (19% of theory).
WORKUP
后处理
- temperatureheated to reflux
- additionwere added
- temperatureunder reflux overnight
- temperatureAfter cooling
- filtrationthe mixture was filtered
- washthe filtercake was washed with a little ethanol
- concentrationthe filtrate was concentrated
- customThe residue was purified by means of preparative HPLC (eluent: acetonitrile/water, gradient 30:70→100:0)