反应详情

Phosphorous oxychloride (1.0 ml) was added to a stirred solution of dimethylacetamide (2.8 ml) in chloroform (10 ml) at room temperature. The mixture was stirred for 5 minutes, 2-cyano-4,5-dimethoxyaniline (1.78 g) added and the reaction stirred under reflux for 4 hours. The mixture was cooled, poured onto ice and extracted with chloroform and the organic phase discarded. The aqueous layer was basified (solid NaOH) extracted with chloroform, the combined extracts washed with water, dried (Na2SO4) and evaporated in vacuo. A sample of the brown oily residue (2 g) was crystallised from diisopropylether to give N,N-dimethyl-N'-(2-cyano-4,5-dimethoxyphenyl)acetamidine, m.p. 94°-96°.

1. stirringthe reaction stirred
2. temperatureunder reflux for 4 hours
3. temperatureThe mixture was cooled
4. additionpoured onto ice
5. extractionextracted with chloroform
6. extractionextracted with chloroform
7. washthe combined extracts washed with water
8. dry with materialdried (Na2SO4)
9. customevaporated in vacuo
10. customA sample of the brown oily residue (2 g) was crystallised from diisopropylether