HRID2278856

反应详情

EQUATION

反应方程式

HRID 2278856 的结构方程式

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

  1. temperatureheated to reflux
  2. additionwere added
  3. temperaturethe mixture was heated
  4. temperatureunder reflux overnight
  5. temperatureAfter cooling
  6. filtrationthe mixture was filtered
  7. washthe filtercake was washed with a little ethanol
  8. custompurified by preparative HPLC (mobile phase: acetonitrile/water with 0.1% TFA, ratio 45:55)