HRID2183551

反应详情

EQUATION

反应方程式

HRID 2183551 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-amino-1-methyl-4-(2,4,6-trimethylphenyl)-1H-pyrrole-2-carbonitrile (2 mmol), methyl acetoacetate (4 mmol) and SnCl4 (4 mmol) in 1,2-dichloroethane was heated at reflux for about six hours until all the starting material were consumed. The mixture was quenched with acetone, basified with saturated NaHCO3, then filtered through Celite?. The filtrate was concentrated to dryness. The residue was quenched with water and extracted with chloroform. The chloroform layer was washed with brine, dried and concentrated to dryness to give 7-amino-1,5-dimethyl-3-(2,4,6-trimethyl-phenyl)-1H-pyrrolo[3,2-b]pyridine-6-carboxylic acid methyl ester. The product may be purified by trituration.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for about six hours until all the starting material
  3. customwere consumed
  4. customThe mixture was quenched with acetone
  5. filtrationfiltered through Celite
  6. concentrationThe filtrate was concentrated to dryness
  7. customThe residue was quenched with water
  8. extractionextracted with chloroform
  9. washThe chloroform layer was washed with brine
  10. customdried
  11. concentrationconcentrated to dryness