HRID2381371

反应详情

EQUATION

反应方程式

HRID 2381371 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5-iodo-2H-pyridazin-3-one (66 g, 0.30 mol) in tetrahydrofuran (500 mL) was treated with pyridinium para-toluene sulfonate (14.3 g, 0.057 mol) and 3,4-dihydro-2H-pyran (52 mL). The reaction mixture was stirred at reflux for 5 h. At this time, the reaction was treated with another aliquot of 3,4-dihydro-2H-pyran (32.5 mL). The solution was stirred at reflux overnight. At this time, the solution was concentrated in vacuo. Chromatography (ethyl acetate/petroleum ether=1/2) afforded 5-iodo-2-(tetrahydro-pyran-2-yl)-2H-pyridazin-3-one (89 g, 98%).

WORKUP

后处理

  1. temperatureat reflux for 5 h
  2. stirringThe solution was stirred
  3. temperatureat reflux overnight
  4. concentrationAt this time, the solution was concentrated in vacuo