HRID399857

反应详情

EQUATION

反应方程式

HRID 399857 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The mixture of methyl 3-(2-formylpyrrol-1-yl)benzoate (3.0 g), malonic acid (2.7 g), pyridine (30 ml) and piperidine (0.3 ml) was stirred for 3 hours at 90°-100° C. The reaction mixture was poured into water, and the mixture was adjusted to pH 1 with 6N-hydrochloric acid. The mixture was extracted with a mixture of ethyl acetate and tetrahydrofuran. The extract layer was washed with brine, dried over magnesium sulfate and evaporated in vacuo. The residue was recrystallized from ethanol to give methyl 3-[2-((E)-2-carboxyethenyl)pyrrol-1-yl)benzoate.

WORKUP

后处理

  1. extractionThe mixture was extracted with a mixture of ethyl acetate and tetrahydrofuran
  2. washThe extract layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residue was recrystallized from ethanol