HRID19892

反应详情

EQUATION

反应方程式

HRID 19892 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4-[3-(2-ethoxycarbonyl-2-oxo-ethyl)-4-nitro-phenoxy]-piperidine-1-carboxylic acid tert-butyl ester (example 43, step 2, 42.25 g, 1.0 eq.), palladium on activated charcoal (10%, 2.111 g, 0.02 eq.) in ethanol (950 mL) was hydrogenated at 30° C. for 9 h. The mixture was filtered, washed with ethanol and evaporated to dryness. The product was recrystallized from ethyl acetate and heptane to yield 25.998 g (69%) as white crystals. MS (m/e): 388.2 (M, 45%).

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. washwashed with ethanol
  3. customevaporated to dryness
  4. customThe product was recrystallized from ethyl acetate and heptane
  5. customto yield 25.998 g (69%) as white crystals