HRID2249407

反应详情

EQUATION

反应方程式

HRID 2249407 的结构方程式

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

4-Carboxy-6-(2,3-dihydro-1-benzofuran-5-yl)-2H-pyridazin-3-one (5.9 g, 22.8 mmol) was suspended in methanol (100 mL), and thionyl chloride (3 g, 25.1 mmol) was added dropwise to the suspension under cooling with ice, followed by stirring for three hours at 80° C. The temperature of the reaction mixture was reduced to room temperature, and the solvent was removed under reduced pressure. Water was added to the residue under cooling on ice, and the formed precipitates were collected through filtration and washed with water, followed by drying, to thereby yield 4.90 g of the title compound as pale yellow micro-needles (78.8%).

WORKUP

后处理

  1. temperatureunder cooling with ice
  2. customwas reduced to room temperature
  3. customthe solvent was removed under reduced pressure
  4. additionWater was added to the residue
  5. temperatureunder cooling on ice
  6. customthe formed precipitates
  7. filtrationwere collected through filtration
  8. washwashed with water
  9. customby drying