HRID1701478

反应详情

EQUATION

反应方程式

HRID 1701478 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

73 g (0.5 mol) of 5-phenyl-2-pyrazoline are hydrogenated in 400 ml of methanol saturated with ammonia with 10 g of freshly prepared Raney nickel for 5 hours at 80° C./100 atmospheres. The Raney nickel is filtered off on a suction filter containing a layer of kieselguhr. The solvent is removed from the filtrate in a rotary evaporator and the residue is distilled in a simple distillation apparatus and then through a 25 cm Vigreux column. This gives 66 g=88% of theory of a colourless oil with a boiling point under 0.0004 mm of 73° C. (literature: boiling point under 21 mm, 138°-141° C.).

WORKUP

后处理

  1. filtrationThe Raney nickel is filtered off on a suction
  2. filtrationfilter
  3. additioncontaining a layer of kieselguhr
  4. customThe solvent is removed from the filtrate in a rotary evaporator
  5. distillationthe residue is distilled in a simple distillation apparatus
  6. customunder 0.0004 mm of 73° C. (literature: boiling point under 21 mm, 138°-141° C.)