HRID569043

反应详情

EQUATION

反应方程式

HRID 569043 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5 g of 4-ethoxycarbonyl indole are added to a solution of 3.1 g of dimethylamino-2-nitroethylene in 20 ml of trifluoroethyl acetate refrigerated under argon. The reaction mixture is introduced into ice water after it had been standing overnight at room temperature. The aqueous phase is repeatedly extracted with ethyl acetate. The combined ethyl acetate extracts are extracted first with sodium bicarbonate solution, then a saturated sodium chloride solution, dried and evaporated. The residue is recrystallized from ethanol. Yield: 4.5 g of 4-ethoxycarbonyl-3-(2-nitrovinyl)-indole. Yellow crystals with a 197°-199° C. melting point.

WORKUP

后处理

  1. extractionThe aqueous phase is repeatedly extracted with ethyl acetate
  2. extractionThe combined ethyl acetate extracts are extracted first with sodium bicarbonate solution
  3. dry with materiala saturated sodium chloride solution, dried
  4. customevaporated
  5. customThe residue is recrystallized from ethanol
  6. customwith a 197°-199° C.