HRID2278856
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
1.098 g (7.035 mmol) of methyl 3,3,3-trifluoro-2-oxopropanoate in 10 ml of ethanol were initially introduced and heated to reflux. Then, 2.000 g (7.035 mmol) of 1-(2-fluorobenzyl)-1H-pyrazolo[3,4-d]pyrimidine-3-carboximidohydrazide suspended in 25 ml of ethanol were added and the mixture was heated under reflux overnight. After cooling, the mixture was filtered, and the filtercake was washed with a little ethanol and purified by preparative HPLC (mobile phase: acetonitrile/water with 0.1% TFA, ratio 45:55). This gave 710 mg of the target compound (purity 93%; 24% of theory).
WORKUP
后处理
- temperatureheated to reflux
- additionwere added
- temperaturethe mixture was heated
- temperatureunder reflux overnight
- temperatureAfter cooling
- filtrationthe mixture was filtered
- washthe filtercake was washed with a little ethanol
- custompurified by preparative HPLC (mobile phase: acetonitrile/water with 0.1% TFA, ratio 45:55)