HRID1195745

反应详情

EQUATION

反应方程式

HRID 1195745 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of methyl 5,6-dihydro-1,2-dioxo-4H-pyrrolo[3,2,1-ij]quinoline-6-carboxylate (Example 1; 3 g)and N-cholorsuccinimide (NCS, 1.96 g) in dimethylformamide (DMF, 30 ml) was heated at 80° C. with stirring for an hour. After cooling, the mixture was concentrated. The residue was extracted with chloroform (200 ml). Chloroform layer was washed with water, dried over anhydrous sodium sulfate and concentrated to give the title compound (3.28 g, 96.2%) which was recrystallized form acetonitrile to dark red needles, mp 132° C.-133° C.

WORKUP

后处理

  1. temperatureAfter cooling
  2. concentrationthe mixture was concentrated
  3. extractionThe residue was extracted with chloroform (200 ml)
  4. washChloroform layer was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated