HRID1181155

反应详情

EQUATION

反应方程式

HRID 1181155 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(3,5-dibromo-4-nitropyrazol-1-yl)propan-2-ol (3-3) (22 g, 666 mmol), EtOH (300 ml) and benzylamine (102 g, 936 mmol) was refluxed for 1.5 hours. The reaction medium was concentrated to the maximum under reduced pressure. DCM (100 ml) was added to the residue. The organic phase was washed with dilute acid (5×50 ml). The organic phase was dried over Na2SO4 and the solvent was evaporated off under reduced pressure. The brown oil obtained was treated with diisopropyl ether at 0° C. to give the 1-(5-benzylamino-3-bromo-4-nitropyrazol-1-yl)propan-2-ol (13.7 g, 58%) in the form of a yellow solid.

WORKUP

后处理

  1. temperaturewas refluxed for 1.5 hours
  2. concentrationThe reaction medium was concentrated to the maximum under reduced pressure
  3. additionDCM (100 ml) was added to the residue
  4. washThe organic phase was washed
  5. additionwith dilute acid (5×50 ml)
  6. dry with materialThe organic phase was dried over Na2SO4
  7. customthe solvent was evaporated off under reduced pressure
  8. customThe brown oil obtained