HRID1244479

反应详情

EQUATION

反应方程式

HRID 1244479 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a 250 ml Parr flask, 2.40 g (6.2 mmoles) of 3,5-bis-(1,1-dimethylethyl)-4-hydroxy-N-[(3-nitrophenyl)methyl]-benzamide is dissolved in 45 ml of an absolute ethanol/TXF mixture (1/2) in the presence of 10% Pd/C. The mixture is agitated under 20 PSI of hydrogen, at 30° C., for three hours. After filtration on celite, the filtrate is concentrated to dryness and the residue is purified on a silica column (eluant: heptane/ethyl acetate: 60/40). The pure fractions are collected and concentrated under reduced pressure to produce 0.94g (45%) of a white powder. Melting point: 171-172° C.

WORKUP

后处理

  1. filtrationAfter filtration on celite
  2. concentrationthe filtrate is concentrated to dryness
  3. customthe residue is purified on a silica column (eluant: heptane/ethyl acetate: 60/40)
  4. customThe pure fractions are collected
  5. concentrationconcentrated under reduced pressure