HRID371430

反应详情

EQUATION

反应方程式

HRID 371430 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4.7 g of m-guanidinobenzoic acid methanesulfonate in 50 ml of anhydrous pyridine, was added 4.4 g of DCC. To the mixture, while being cooled in ice and stirred, was added 5.0 g of 6-amidino-2-naphthol methanesulfonate. After having been stirred for 24 hours, the reaction mixture was freed from the insolubles by filtration and the filtrate was mixed with ether. The oily substance which was formed was crystallized by adding ethyl acetate. Recrystallization from a mixture of methanol and ether gave 3.2 g of 6-amidino-2-naphthyl 3-guanidinobenzoate dimethanesulfonate.

WORKUP

后处理

  1. temperatureTo the mixture, while being cooled in ice
  2. stirringAfter having been stirred for 24 hours
  3. filtrationthe reaction mixture was freed from the insolubles by filtration
  4. additionthe filtrate was mixed with ether
  5. customThe oily substance which was formed
  6. customwas crystallized
  7. additionby adding ethyl acetate
  8. customRecrystallization
  9. additionfrom a mixture of methanol and ether