反应详情

A solution of 11 g of N-(4-pyridyl)ethylenediamine and 5.3 g of 2-nitrocinnamyl chloride (trans-form) dissolved in 60 ml of ethanol was stirred at room temperature for 30 minutes and then stirred at 50° C. for 90 minutes. The solvent was distilled off under reduced pressure, and 10% aqueous sodium hydroxide was added to the residue and the mixture was extracted with chloroform. After drying of the extract, chloroform was distilled off and the residue was purified by silica gel column chromatography (solvent: chloroform-methanol-triethylamine=20:1:0.1) to give 2.33 g of (E)-N-(2-nitrocinnamyl)-N'-(4-pyridyl)ethyenediamine as a yellow oily substance.

1. stirringstirred at 50° C. for 90 minutes
2. distillationThe solvent was distilled off under reduced pressure, and 10% aqueous sodium hydroxide
3. additionwas added to the residue
4. extractionthe mixture was extracted with chloroform
5. dry with materialAfter drying of the extract, chloroform
6. distillationwas distilled off
7. customthe residue was purified by silica gel column chromatography (solvent: chloroform-methanol-triethylamine=20:1:0.1)