反应详情

In a 500 ml round bottomed flask equipped with a reflux condensor was placed 100 g of 3-dimethylamino-2-methyl-4'-chloropropiophenone (0.47 mole), 200 ml of n-propanol, 48 g of hydrazine monohydrate (0.96 mole), and 5 g of 50% aqueous sodium hydroxide. The mixture was refluxed for 2 hours. The solvent was removed in vacuo and the product was partitioned between methylene chloride and water. The organic layer was washed 3 times with water and dried over anyhdrous magnesium sulfate. The organic layer contains 82 g (0.42 mole) of 3-(4-chlorophenyl)-4-methyl-4,5-dihydro-1H-pyrazole an air sensitive solid. NMR data was consistent with the structure.

1. customIn a 500 ml round bottomed flask equipped with a reflux condensor
2. temperatureThe mixture was refluxed for 2 hours
3. customThe solvent was removed in vacuo
4. customthe product was partitioned between methylene chloride and water
5. washThe organic layer was washed 3 times with water
6. dry with materialdried over anyhdrous magnesium sulfate