反应详情

温度

40 °C

Into a 50 milliliter glass reactor equipped with a thermometer connected to a temperature controller, a heating mantle, a condenser and a magnetic stirring bar, is charged 9 gms (0.0215 mole) of 4-methoxybenzyl triphenyl phosphonium chloride and 25 gms of acetic acid. The mixture is heated to 40° C. then 1 gm (0.0588 mole) of ammonia is added. This reaction mass is heated to 80° C. and maintained there for 1.17 hours, then heated to 100° C. and maintained thereat for 18 hours, then heated to 110° C. and maintained thereat 4.8 hours, and then cooled to 30° C. To this is added 40 g of benzene and the contents let stand overnight to settle the solids, then the liquid is removed by decantation and vacuum distillation to obtain 7.8 g of product having a melting point of 121° C. to 130° C.

1. customInto a 50 milliliter glass reactor equipped with a thermometer
2. temperatureThis reaction mass is heated to 80° C.
3. temperaturemaintained there for 1.17 hours
4. temperatureheated to 100° C.
5. temperaturemaintained
6. temperatureheated to 110° C.
7. temperaturemaintained
8. temperature4.8 hours, and then cooled to 30° C
9. waitthe contents let stand overnight
10. customthe liquid is removed by decantation and vacuum distillation