HRID797

反应详情

EQUATION

反应方程式

HRID 797 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
23 °C

PROCEDURE

实验过程

4,5-Dibromo-2-methyl-3(2H)-pyridazinone (20 g, Maybridge Chemical Company) was cooled in an ice bath and treated successively with methanol (200 mL) and sodium methoxide (12 mL of a 30% solution in methanol). The ice bath was removed and the reaction was allowed to stir at 23° C. for 3 h. The methanol was removed by evaporation at reduced pressure. The residue was partitioned between dichloromethane and water. The organic layer was dried over magnesium sulfate and concentrated to provide the desired product 17 g as a whim solid melting at 146°-147° C. 1 H NMR (CDCl3): 7.7 (1H), 4.0 (3H), 3.8 (3H).

WORKUP

后处理

  1. customThe ice bath was removed
  2. customThe methanol was removed by evaporation at reduced pressure
  3. customThe residue was partitioned between dichloromethane and water
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. concentrationconcentrated