HRID1072707

反应详情

EQUATION

反应方程式

HRID 1072707 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-[1-[2-(4-bromophenyl)ethan-1-yl]-5-methyl-1H-pyrrol-2-yl]phenol (3.00 g, 8.42 mmol), ethyl (S)-2-hydroxy-3-phenylpropanoate (1.96 g, 10.1 mmol) and triphenylphosphine (2.65 g, 10.1 mmol) in toluene (30 ml) was added diethyl azodicarboxylate (1.76 g, 10.1 mmol) and refluxed for 20 hours under heating. The insoluble matter was filtered out and the filtrate was diluted with ethyl acetate. The obtained solution was washed with water and dried over magnesium sulfate anhydride, and the solvent was removed under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=8:1) to give the object compound as an oily substance. 2.40 g (yield: 54.0%)

WORKUP

后处理

  1. temperaturerefluxed for 20 hours
  2. temperatureunder heating
  3. filtrationThe insoluble matter was filtered out
  4. additionthe filtrate was diluted with ethyl acetate
  5. washThe obtained solution was washed with water
  6. dry with materialdried over magnesium sulfate anhydride
  7. customthe solvent was removed under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=8:1)
  9. customto give the object compound as an oily substance