HRID1181155
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas refluxed for 1.5 hours
- concentrationThe reaction medium was concentrated to the maximum under reduced pressure
- additionDCM (100 ml) was added to the residue
- washThe organic phase was washed
- additionwith dilute acid (5×50 ml)
- dry with materialThe organic phase was dried over Na2SO4
- customthe solvent was evaporated off under reduced pressure
- customThe brown oil obtained