HRID2233207

反应详情

EQUATION

反应方程式

HRID 2233207 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 3-ethenyl-6,7-dihydro-5H-pyrano[2,3-c]pyridazine (100 mg, 0.617 mmol) in 1,4-dioxane (5.5 ml)/water (1.1 ml) was cooled in ice/water and treated with sodium periodate (306 mg, 1.43 mmol) and a 4% aqueous solution of osmium tetroxide (0.55 ml). The mixture was allowed to warm to RT after an hour, and after a total of 4.75 hours stirring, the solvent was evaporated. 1,4-Dioxane was added and evaporated, a few ml of dichloromethane were added and the mixture briefly held in an ultrasonic bath. The whole mixture was applied to a silica column and eluted with ethyl acetate to give the product (55 mg, 54%).

WORKUP

后处理

  1. customthe solvent was evaporated
  2. addition1,4-Dioxane was added
  3. customevaporated
  4. additiona few ml of dichloromethane were added
  5. customthe mixture briefly held in an ultrasonic bath
  6. washeluted with ethyl acetate