HRID1761927

反应详情

EQUATION

反应方程式

HRID 1761927 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1.90 g of methyl 3-formyl-2-hydroxybenzoate, 3.0 g of nitroethane, 0.15 ml of piperidine and 30 ml of toluene is refluxed overnight while removing water. The reaction mixture is poured into ice-water and the aqueous mixture is extracted with ethyl acetate. The extract is washed successively with 10% hydrochloric acid and an aqueous saturated sodium chloride solution, dried and evaporated to remove solvent. The residue is recrystallized from methanol to give 2.05 g of methyl 2-hydroxy-3-(2-nitro-1-propenyl)benzoate.

WORKUP

后处理

  1. temperatureis refluxed overnight
  2. customwhile removing water
  3. additionThe reaction mixture is poured into ice-water
  4. extractionthe aqueous mixture is extracted with ethyl acetate
  5. washThe extract is washed successively with 10% hydrochloric acid
  6. dry with materialan aqueous saturated sodium chloride solution, dried
  7. customevaporated
  8. customto remove solvent
  9. customThe residue is recrystallized from methanol