HRID570530

反应详情

EQUATION

反应方程式

HRID 570530 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureheated to reflux
  2. additionwere added
  3. temperatureunder reflux overnight
  4. temperatureAfter cooling
  5. filtrationthe mixture was filtered
  6. washthe filtercake was washed with a little ethanol
  7. concentrationthe filtrate was concentrated
  8. customThe residue was purified by means of preparative HPLC (eluent: acetonitrile/water, gradient 30:70→100:0)