反应详情

A 250 ml 3-neck flask was equipped with an overhead stirrer, thermocouple, reflux condenser and heating mantle. The flask was charged with (E)-2-acetyl-3-dimethylamino-acrylonitrile (8.93 g, 63.34 mmol), N-tert-butyloxycarbonyl-guanidine (10 g, 61.56 mmol) and 2-methyltetrahydrofuran (98.76 g). The resultant suspension was stirred and heated to reflux, whereupon the solids were observed to dissolve. The resultant mixture was stirred for about 6 hours, then concentrated by rotary evaporation to yield a solid which was triturated with water (120.00 g) to complete precipitation of the desired product. The resultant suspension was stirred for ˜30 minutes at ambient temperature, then filtered and the wet solid washed twice with water (120.00 g) and dried in a vacuum oven at 75-80° C. under a N2 bleed overnight to yield the title compound.

1. customA 250 ml 3-neck flask was equipped with an overhead stirrer
2. temperaturethermocouple, reflux condenser
3. temperatureheating mantle
4. temperatureheated
5. temperatureto reflux, whereupon the solids
6. dissolutionto dissolve
7. concentrationconcentrated by rotary evaporation
8. customto yield a solid which
9. customwas triturated with water (120.00 g)
10. customprecipitation of the desired product
11. filtrationfiltered
12. washthe wet solid washed twice with water (120.00 g)
13. customdried in a vacuum oven at 75-80° C. under a N2
14. waitbleed overnight