HRID43297

反应详情

EQUATION

反应方程式

HRID 43297 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

180 g (0.453 mol) of 3-{4-[(2-butyl-5-nitro-1-benzofuran-3-yl) carbonyl]phenoxy}propan-1-ol (formula(II)) dissolved in 1800 ml of methanol are loaded in a glass Buchi autoclave. Subsequently 9 g of Pd/C 10% (50% H2O) are added and H2 is loaded at a pressure of 4 bars. The mixture is left under stirring maintaining the temperature below 40° C. Once the consumption of hydrogen is complete, the reaction is left under stirring for approximately one further hour until it reaches 25° C. The catalyst is filtered on a Celite panel and the alcoholic solution containing the product is concentrated to residue. The crude product is crystallised, recovering it with 400 ml of toluene and the product is dried under a vacuum at 40° C. for 6-7 hours. 151 g of the product in the title are obtained.

WORKUP

后处理

  1. waitThe mixture is left
  2. temperaturemaintaining the temperature below 40° C
  3. customOnce the consumption of hydrogen
  4. waitthe reaction is left
  5. stirringunder stirring for approximately one further hour until it
  6. customreaches 25° C
  7. filtrationThe catalyst is filtered on a Celite panel
  8. additionthe alcoholic solution containing the product
  9. concentrationis concentrated to residue
  10. customThe crude product is crystallised
  11. customrecovering it with 400 ml of toluene
  12. customthe product is dried under a vacuum at 40° C. for 6-7 hours