HRID351262

反应详情

EQUATION

反应方程式

HRID 351262 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 10% Pd-C 50% wet (100 mg) and ethyl 5-(4-cyanophenyl)-1-(4-methoxyphenyl)-1H-pyrazole-3-carboxylate (1 g) in THF (10 ml), MeOH (5 ml), and 1M HCl (2.9 ml) was hydrogenated under H2 latmat ambient temperature for 6.5 hours. The catalyst was filtered off through a celite pad and the pad was washed with MeOH. The filtrate and combined washings were concentrated in vacuo. The residue was dissolved in EtOH and concentrated in vacuo. The residue was crystallized from AcOEt to give ethyl 5-[4-(aminomethyl)phenyl]-1-(4-methoxyphenyl)-1H-pyrazole-3-carboxylate hydrochloride (984 mg) as a powder.

WORKUP

后处理

  1. filtrationThe catalyst was filtered off through a celite pad
  2. washthe pad was washed with MeOH
  3. concentrationwere concentrated in vacuo
  4. dissolutionThe residue was dissolved in EtOH
  5. concentrationconcentrated in vacuo
  6. customThe residue was crystallized from AcOEt