HRID653072

反应详情

EQUATION

反应方程式

HRID 653072 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

1-{2-Hydroxy-3-propyl-4-[3-(4-nitrophenoxy)propoxy]phenyl}ethanone (19.6 g) was dissolved in a mixture of ethanol (300 ml) and dimethylformamide (100 ml), to which was added under nitrogen, a slurry of palladium on charcoal catalyst (1.0 g, 5%) in ethanol (50 ml). The suspension was then hydrogenated on a Parr at 60 psi and room temperature for 90 minutes. The suspension was filtered over Celite (registered Trade Mark), washed with ethanol and the filtrate evaporated under reduced pressure to a brown oil, which was triturated with water and filtered to give a brown solid. The solid was recrystallised from ethanol with charcoal to give a white solid, m.p. 75°-77° C.

WORKUP

后处理

  1. additionwas added under nitrogen
  2. filtrationThe suspension was filtered over Celite (registered Trade Mark)
  3. washwashed with ethanol
  4. customthe filtrate evaporated under reduced pressure to a brown oil, which
  5. customwas triturated with water
  6. filtrationfiltered
  7. customto give a brown solid
  8. customThe solid was recrystallised from ethanol with charcoal
  9. customto give a white solid, m.p. 75°-77° C.