HRID444538

反应详情

EQUATION

反应方程式

HRID 444538 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the solution of 52 g of ethyl 4-nitrophenylacetate in 350 ml dimethylformamide-toluene (1:1), 9.5 g of 50% sodium hydride in mineral oil are added portionwise while stirring and cooling. After 11/2 hours stirring at room temperature, 26 g methyl iodide are added dropwise and the mixture is stirred overnight at room temperature. The mixture is carefully combined with water, extracted with diethyl ether, the extract dried, filtered and evaporated. The residue is taken up in 100 ml ethanol, the solution seeded with a few crystals starting material and allowed to stand in the cold. The precipitate formed is filtered off and the filtrate evaporated, to yield the ethyl α-(4-nitrophenyl)-propionate.

WORKUP

后处理

  1. temperaturecooling
  2. stirringAfter 11/2 hours stirring at room temperature
  3. stirringthe mixture is stirred overnight at room temperature
  4. extractionextracted with diethyl ether
  5. customthe extract dried
  6. filtrationfiltered
  7. customevaporated
  8. customThe precipitate formed
  9. filtrationis filtered off
  10. customthe filtrate evaporated