HRID55434

反应详情

EQUATION

反应方程式

HRID 55434 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 0.85 g of (3aS,4S, 6R, 7aR)-2-[2-(S)-(2-benzoxyphenyl) propionyl]-4-(2-methoxyphenyl)-6-methyl-4-perhydroisoindolol in 12 cm3 of absolute ethanol is added 0.2 g of 20% palladium hydroxide on charcoal, and hydrogen is sparged through the reaction mixture at 40° C. for 3 hours. After returning to room temperature and flushing with argon, the mixture is filtered over fire and concentrated to dryness under reduced pressure (2.7 kPa). The residue is recrystallized in ethanol and, after filtration and drying, 0.5 g of (3aS,4S,6R,7aR)-2-(S)-(2-hydroxyphenyl) propionyl]-4-(2-methoxtphenyl)-6-methyl-4-perhydroisoindolol is obtained, in the form of white crystals melting at 280° C.; [α]D =-26.5° (c=5.3 g/l , CHCl3).

WORKUP

后处理

  1. customis sparged through the reaction mixture at 40° C. for 3 hours
  2. customAfter returning to room temperature
  3. customflushing with argon
  4. filtrationthe mixture is filtered over fire
  5. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)
  6. customThe residue is recrystallized in ethanol
  7. filtrationafter filtration
  8. customdrying