HRID15153

反应详情

EQUATION

反应方程式

HRID 15153 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[1,4]oxathiino[2,3-c]pyridazine (320 mg) in 1,4-dioxane/water (20 ml/5 ml) was treated with an aqueous solution of osmium tetroxide (4% w/v, 2 ml) and sodium periodate (1.08 g), initially stirred in an ice-bath, then allowed to warm to room temperature. After 2.5 hours the mixture was evaporated to dryness and dissolved in 1,4-dioxane and chloroform. Silica gel was added and the mixture was evaporated to dryness, added to a silica column (50 g) and chromatographed, eluting with 0-100% ethyl acetate in hexane, to afford a white solid (116 mg, 36%).

WORKUP

后处理

  1. customAfter 2.5 hours the mixture was evaporated to dryness
  2. dissolutiondissolved in 1,4-dioxane
  3. additionSilica gel was added
  4. customthe mixture was evaporated to dryness
  5. additionadded to a silica column (50 g)
  6. customchromatographed
  7. washeluting with 0-100% ethyl acetate in hexane