HRID1713039

反应详情

EQUATION

反应方程式

HRID 1713039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The resulting azide, 2-azido-3-thiophen-2-yl-acrylic acid ethyl ester (650 mg, 2.88 mmol) was dissolved in toluene (40 ml) and the solution was refluxed for 2 hours. The solution was thereafter cooled, and water (80 ml) was added. After separation of the phases the aqueous phase was extracted with ethyl acetate (3×20 ml), the combined organic phase was dried over Na2SO4 and the organic solvents were evaporated under reduced pressure. The crude product was purified by silica gel flash chromatography to give 450 mg of pure 4H-thieno[3,2-b]pyrrole-5-carboxylic acid ethyl ester (80% yield).

WORKUP

后处理

  1. temperaturethe solution was refluxed for 2 hours
  2. temperatureThe solution was thereafter cooled
  3. customAfter separation of the phases the aqueous phase
  4. extractionwas extracted with ethyl acetate (3×20 ml)
  5. dry with materialthe combined organic phase was dried over Na2SO4
  6. customthe organic solvents were evaporated under reduced pressure
  7. customThe crude product was purified by silica gel flash chromatography