HRID1029869

反应详情

EQUATION

反应方程式

HRID 1029869 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(3aRS,7aRS)-2-benzyl-7,7-diphenyl-4-perhydroisoindolone (150 g), methanol (1,500 cc) and 1N hydrochloric acid (450 cc) are added to 10% palladiumon-charcoal (15 g); the reaction mixture is hydrogenated, with stirring, at ambient temperature and under atmospheric pressure. After a reaction time of 5 hours, the theoretical volume of hydrogen has been absorbed; the reaction mixture is filtered and the filtrate is then concentrated to dryness under reduced pressure (2.7 kPa); the residue is crystallized from ethanol (200 cc); the crystals obtained are drained, washed with ethanol (50 cc) and dried. (3aRS,7aRS)-7,7-diphenyl-4-perhydroisoindolone hydrochloride (110 g) melting at 270° C. with decomposition is obtained.

WORKUP

后处理

  1. customAfter a reaction time of 5 hours, the theoretical volume of hydrogen has been absorbed
  2. filtrationthe reaction mixture is filtered
  3. concentrationthe filtrate is then concentrated to dryness under reduced pressure (2.7 kPa)
  4. customthe residue is crystallized from ethanol (200 cc)
  5. customthe crystals obtained
  6. washwashed with ethanol (50 cc)
  7. customdried