反应详情

温度

91 °C

To a 1 liter flask was charged 206.5 g (0.7 mole) of alpha-(2,4-dichlorophenyl)-alpha-ethyl-1H-1,2,4-triazole-1-propanenitrile and 500 mL of dimethyl sulfoxide and 200 mL of water. To the stirring solution was added 67.2 g (0.84 moles) of 50% sodium hydroxide. The reaction mixture was heated at 91 ° C. (steam bath) for 3 hours after which GLC indicated the starting material was consumed. The reaction was cooled to 30° C. then poured into water and extracted with ethyl acetate. After drying, the ethyl acetate was treated with charcoal and filtered through Celite®. Removal of the solvent gave a foamy oil which was stirred and diluted with ethyl acetate then treated with hexane until cloudy. Within 1 hour a solid formed which was cooled at 0° C. The product was filtered and washed with an ether and hexane mixture, then dried and provided 172 g (79% yield) of a white solid, melting point 164°-165° C.

1. customwas consumed
2. temperatureThe reaction was cooled to 30° C.
3. additionthen poured into water
4. extractionextracted with ethyl acetate
5. customAfter drying
6. additionthe ethyl acetate was treated with charcoal
7. filtrationfiltered through Celite®
8. customRemoval of the solvent
9. customgave a foamy oil which
10. customWithin 1 hour a solid formed which
11. temperaturewas cooled at 0° C
12. filtrationThe product was filtered
13. washwashed with an ether and hexane mixture
14. customdried