HRID1701478
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationThe Raney nickel is filtered off on a suction
- filtrationfilter
- additioncontaining a layer of kieselguhr
- customThe solvent is removed from the filtrate in a rotary evaporator
- distillationthe residue is distilled in a simple distillation apparatus
- customunder 0.0004 mm of 73° C. (literature: boiling point under 21 mm, 138°-141° C.)