HRID329635

反应详情

EQUATION

反应方程式

HRID 329635 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 13.5 g of -N-methyl-N-[3-(3-methyl-1,2,4-triazolo[4,3-b]-pyridazin-6-yl)phenyl]acetamide and 10 g of potassium hydroxide in 500 ml of ethanol was heated to reflux for 12 hours. The solution was concentrated in vacuo and the residue partitioned between 200 ml of brine and 300 ml dichloromethane. The aqueous layer was extracted with 150 ml portions of dichloromethane. The combined organic layer and extracts were dried, concentrated in vacuo and the residue recrystalized from dichloromethanehexane, to give 11.66 g of yellow crystals, mp 223°-226° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 12 hours
  3. concentrationThe solution was concentrated in vacuo
  4. customthe residue partitioned between 200 ml of brine and 300 ml dichloromethane
  5. extractionThe aqueous layer was extracted with 150 ml portions of dichloromethane
  6. customThe combined organic layer and extracts were dried
  7. concentrationconcentrated in vacuo
  8. customthe residue recrystalized from dichloromethanehexane