HRID1065369

反应详情

EQUATION

反应方程式

HRID 1065369 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.87 gm of 2,3-dichloro-5,6-dicyano-benzoquinone were added to a solution of 1.8 gm of 5-(4-phenylsulfonyl-butoxy)-3,4-dihydro-carbostyril in 45 ml of dioxane, and the solution was boiled for 2.5 hours on an oil bath. The reaction mixture was then filtered while still hot, and the insoluble matter, which was formed during the reaction was washed with hot dioxane. The combined filtrates were diluted with 100 ml of chloroform and extracted several times with altogether 150 ml of 2N sodium hydroxide. After drying the chloroform extracts with sodium sulfate and filtering in the presence of activated charcoal, the filtrate was concentrated by evaporation, and ethyl acetate was added until white crystals were precipitated.

WORKUP

后处理

  1. filtrationThe reaction mixture was then filtered while still hot, and the insoluble matter
  2. customwhich was formed during the reaction
  3. washwas washed with hot dioxane
  4. additionThe combined filtrates were diluted with 100 ml of chloroform
  5. extractionextracted several times with altogether 150 ml of 2N sodium hydroxide
  6. dry with materialAfter drying the chloroform
  7. filtrationfiltering in the presence of activated charcoal
  8. concentrationthe filtrate was concentrated by evaporation, and ethyl acetate
  9. additionwas added until white crystals
  10. customwere precipitated