HRID1730947

反应详情

EQUATION

反应方程式

HRID 1730947 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Phthalimidopropyl-3-phenyl-5-chloroindazole (8.3 g) and hydrazine hydrate (2.0 g) were added to ethanol (150 ml) followed by heating under reflux for 3 hours. The reaction mixture was concentrated under reduced pressure and to the residue were added benzene (150 ml) and 10% aqueous sodium hydroxide solution (200 ml) followed by stirring at room temperature for 1 hour. The organic layer was separated from the mixture and it was washed with water, dried over sodium sulfate and concentrated under reduced pressure to obtain 5.5 g of 1-aminopropyl-3-phenyl-5-chloroindazole as an oily product. The product was treated with ether-hydrochloric acid to form its hydrochloride. After recrystallization from ethanol-ether, the product had a melting point between 163°-164° C.

WORKUP

后处理

  1. temperatureby heating
  2. temperatureunder reflux for 3 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure and to the residue
  4. additionwere added benzene (150 ml) and 10% aqueous sodium hydroxide solution (200 ml)
  5. customThe organic layer was separated from the mixture and it
  6. washwas washed with water
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated under reduced pressure