HRID636418
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
2.05 ml (40.9 mmol) of NH2NH2 were added to a solution of 9.08 g (38.3 mmol) of 2-benzenesulphonyl-3-dimethylamino-acrylonitrile in 60 ml of EtOH and stirred at 40° for 5 hrs. The reaction solution was evaporated and the residue was partitioned between H2O and CH2Cl2. The aqueous phase was washed three times with CH2Cl2, and the combined organic phases were dried (MgSO4), filtered and evaporated. Chromatography (SiO2, CH2Cl2/MeOH 10:1) yielded 2.5 g (30%) of 4-benzenesulphonyl-1H-pyrazol-3-ylamine as a beige powder, m.p. 159-161°.
WORKUP
后处理
- customThe reaction solution was evaporated
- customthe residue was partitioned between H2O and CH2Cl2
- washThe aqueous phase was washed three times with CH2Cl2
- dry with materialthe combined organic phases were dried (MgSO4)
- filtrationfiltered
- customevaporated