HRID1744174

反应详情

EQUATION

反应方程式

HRID 1744174 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of [2-(5-benzylamino-3-bromo-4-nitropyrazol-1-yl)ethyl]carbamic acid tert-butyl ester (2.1 g; 4.76 mmol) in EtOH (100 ml) containing a 5% Pd/C catalyst (Engelhard type, 50% moisture, 0.4 g wet weight) was hydrogenated in an autoclave (250 ml) at 15 bar for 3 h. The catalyst was filtered off under an inert atmosphere and washed with EtOH, and the filtrate was recovered in an ethanolic solution (25 ml) containing hydrobromic acid (47%, 2 ml). The orange-colored solution was evaporated to dryness to give the 2-(2-aminoethyl)-2H-pyrazole-3,4-diamine in the hydrobromide form (3.55 HBr) as a pale pink solid (1.5 g, 92%).

WORKUP

后处理

  1. filtrationThe catalyst was filtered off under an inert atmosphere
  2. washwashed with EtOH
  3. customthe filtrate was recovered in an ethanolic solution (25 ml)
  4. additioncontaining hydrobromic acid (47%, 2 ml)
  5. customThe orange-colored solution was evaporated to dryness