HRID2381326

反应详情

EQUATION

反应方程式

HRID 2381326 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-(2-acetyl-phenoxy)-4-chloro-2-(tetrahydro-pyran-2-yl)-2H-pyridazin-3-one (15.0 g, 0.043 mol), concentrated hydrochloric acid (30 mL), water (45 mL) and methanol (130 mL) was heated at reflux for 2 h. At this time, the reaction was concentrated in vacuo. The residue was charged with water (200 mL) and then basified with a saturated aqueous sodium bicarbonate solution. The resulting material was collected by filtration, rinsed with water and petroleum ether, and dried to afford 5-(2-acetyl-phenoxy)-4-chloro-2H-pyridazin-3-one (9.0 g, 79%); ESI-MS 265 [M+H+].

WORKUP

后处理

  1. temperatureat reflux for 2 h
  2. concentrationAt this time, the reaction was concentrated in vacuo
  3. additionThe residue was charged with water (200 mL)
  4. filtrationThe resulting material was collected by filtration
  5. washrinsed with water and petroleum ether
  6. customdried