HRID839308

反应详情

EQUATION

反应方程式

HRID 839308 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.6 g. of 3-amino-4-chloro-α-ethyl-benzhydrol are dissolved in methanol containing 3.9 g of potassium hydroxide. 8.7 g. of an 5% palladium-on-calcium carbonate catalyst are added to the mixture, and the suspension is hydrogenated at room temperature under atmospheric pressure. After the uptake of the calculated amount of hydrogen the catalyst is filtered off and washed with 15 ml. of methanol. The filtrate and the wash are combined and concentrated to 40 ml. under reduced pressure. The product is precipitated from the concentrate with water. The solids are filtered off, washed until neutral, and dried until constant weight. The crude product is recrystallized from alcohol to yield 1.7 g. of 3 amino-α-ethyl-benzhydrol, melting at 92-93° C.

WORKUP

后处理

  1. customis hydrogenated at room temperature under atmospheric pressure
  2. filtrationAfter the uptake of the calculated amount of hydrogen the catalyst is filtered off
  3. washwashed with 15 ml
  4. concentrationconcentrated to 40 ml
  5. customThe product is precipitated from the
  6. concentrationconcentrate with water
  7. filtrationThe solids are filtered off
  8. washwashed until neutral, and
  9. customdried until constant weight
  10. customThe crude product is recrystallized from alcohol
  11. customto yield 1.7 g