反应详情

温度

5 °C

A mixture of 15.8 g of 4-cyanophenoxyacetonitrile and 23.3 g of ethylenediamine p-toluenesulfonate in 50 ml of 1,2-dichlorobenzene was heated at from about 130°-145° C. for about an hour. After reaction the mixture was cooled, diluted with CH2Cl2 and filtered to obtain the crude product. The crude product was dissolved in boiling absolute ethanol, treated with activated charcoal and filtered through a fluted paper. The filtrate was cooled to 5° C. for 1.5 hours and the crystals which formed removed by filtering. After drying in a vacuum oven, off-white crystals were obtained having a melting point of 190°-192° C. The off-white crystals were put in solution in 200 ml of boiling water and treated with activated charcoal and filtered. The filtrate was cooled to 5° C. for 1 hour and the crystals which formed removed by filtration. Upon drying, the product 2-((4-cyanophenoxy)methyl)-2-imidazoline p-toluenesulfonate was obtained as white crystals, m.p. 196°-198° C.

1. temperaturewas heated at from about 130°-145° C. for about an hour
2. customAfter reaction the mixture
3. temperaturewas cooled
4. filtrationfiltered
5. customto obtain the crude product
6. filtrationfiltered through a fluted paper
7. customthe crystals which formed
8. customremoved
9. filtrationby filtering
10. customAfter drying in a vacuum oven
11. customoff-white crystals were obtained
12. filtrationfiltered
13. temperatureThe filtrate was cooled to 5° C. for 1 hour
14. customthe crystals which formed
15. customremoved by filtration
16. customUpon drying