HRID247584

反应详情

EQUATION

反应方程式

HRID 247584 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 30 ml of methanol was dissolved 3.3 g of N-(2-aminoethyl)-5-isoquinolinesulfonamide obtained in Referential example 1, and to the solution was added 25 ml of water solution containing 5.0 g of S-methylisothiourea sulfate. And to the mixed solution was added 1N aqueous sodium hydroxide solution, the mixed solution thus obtained was heated at reflux for two hours. After the reflux, the methanol was distilled therefrom under reduced pressure, and the white crystals precipitated were separated by filtration under reduced pressure. The crystalline residue thus obtained was recrystallized from methanol to give 3.24 g of N-(2-guanidinoethyl)-5-isoquinolinesulfonamide, i.e., Compound (2) in a yield of 84%.

WORKUP

后处理

  1. customobtained in Referential example 1
  2. customthe mixed solution thus obtained
  3. temperaturewas heated
  4. temperatureat reflux for two hours
  5. distillationAfter the reflux, the methanol was distilled
  6. customunder reduced pressure, and the white crystals precipitated
  7. customwere separated by filtration under reduced pressure
  8. customThe crystalline residue thus obtained
  9. customwas recrystallized from methanol