HRID2394979

反应详情

EQUATION

反应方程式

HRID 2394979 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

200 g (0.69 mole) of hydrochloride (2) were dissolved in one litre of concentrated hydrochloric acid and allowed to stand at room temperature. The hydrochloric acid was removed by distillation under vacuum. The residue was dissolved in 1 l of ice-water and the pH was adjusted to 13 with 10 molar sodium hydroxide solution. After extraction with ether, drying the organic phase and removing the solvent by distillation, 162 g of crude product were obtained, and were purified by recrystallisation. 79 g (42% theoretical) of hydrochloride (1) with a melting point of 169°-170° C. were obtained.

WORKUP

后处理

  1. customto stand at room temperature
  2. customThe hydrochloric acid was removed by distillation under vacuum
  3. dissolutionThe residue was dissolved in 1 l of ice-water
  4. extractionAfter extraction with ether
  5. customdrying the organic phase
  6. customremoving the solvent
  7. distillationby distillation
  8. custom162 g of crude product were obtained
  9. customwere purified by recrystallisation