HRID461295
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 0.18 mole of 4-methoxy-phenylhydrazine, 0.27 mole of methyl isopropylketone, 5 drops of acetic acid and 300 ml of ethanol was refluxed for 3 h, whereupon the solvent was evaporated. The dark residue (28 g of hydrazone) was dissolved in 125 ml of ethanol. After adding 54 ml of a 15% by weight solution of concentrated sulphuric acid in ethanol the mixture was refluxed for 2.5 h. The white precipitate (ammonium sulphate) was filtered and the filtrate was diluted with 750 ml of water, neutralized with a few ml of aqueous 5N sodium hydroxide and extracted with ether. The dried extract was distilled in vacuo. Boiling point: 138°-142° C/8 mm Hg.
WORKUP
后处理
- temperaturewas refluxed for 3 h, whereupon the solvent
- customwas evaporated
- dissolutionThe dark residue (28 g of hydrazone) was dissolved in 125 ml of ethanol
- additionAfter adding 54 ml of a 15% by weight solution of concentrated sulphuric acid in ethanol the mixture
- temperaturewas refluxed for 2.5 h
- filtrationThe white precipitate (ammonium sulphate) was filtered
- additionthe filtrate was diluted with 750 ml of water
- extractionextracted with ether
- extractionThe dried extract
- distillationwas distilled in vacuo