HRID1969934

反应详情

EQUATION

反应方程式

HRID 1969934 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

30 μL (0.37 mmol) of pyridine and 20 μL (0.22 mmol) of aniline are added to 60 mg (0.18 mmol) of 8-chlorosulfonyl-4-oxo-4,5-dihydro-3H-pyrrolo[2,3-c]quinoline-1-carboxylic acid suspended in 4 mL of anhydrous dichloromethane and 1 mL of anhydrous dimethylformamide. The reaction mixture is stirred for 5 hours at room temperature then diluted with a 10% aqueous solution of potassium carbonate and dichloromethane. The phases are separated and the aqueous phase is acidified with acetic acid to pH of 4. The product is extracted with dichloromethane. The organic phase is dried over magnesium sulfate, filtered then evaporated. The residue is diluted with water (5 mL) then the solid is filtered and dried under vacuum to give 30 mg (42%) of 4-oxo-8-phenylsulfamoyl-4,5-dihydro-3H-pyrrolo[2,3-c]quinoline-1-carboxylic acid in the form of a beige solid.

WORKUP

后处理

  1. customThe phases are separated
  2. extractionThe product is extracted with dichloromethane
  3. dry with materialThe organic phase is dried over magnesium sulfate
  4. filtrationfiltered
  5. customthen evaporated
  6. additionThe residue is diluted with water (5 mL)
  7. filtrationthe solid is filtered
  8. customdried under vacuum