HRID1896768

反应详情

EQUATION

反应方程式

HRID 1896768 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 2-chloro-5-nitrobenzo[d]oxazole (404 mg, 2.04 mmol), 2-(tributylstannyl)-thiophene (648 μL, 2.04 mmol) and tetrakis(triphenylphosphine)palladium (0) (40.8 mg) in dioxane (12.2 mL) was heated at 100° C. for 16 h under nitrogen. Ethyl acetate was added, the organic layer was washed with water, dried over anhydrous MgSO4 and evaporated. The resulting solid was purified by column chromatography eluting with ethyl acetate/hexanes 10:90 v/v, and then purified by reverse phase HPLC to afford 3 mg (2%) of the title product (LCMS RT=6.95 min)

WORKUP

后处理

  1. washthe organic layer was washed with water
  2. dry with materialdried over anhydrous MgSO4
  3. customevaporated
  4. customThe resulting solid was purified by column chromatography
  5. washeluting with ethyl acetate/hexanes 10:90 v/v
  6. custompurified by reverse phase HPLC