反应详情

温度

40 °C

A 1 L Pyrex glass, four-neck, round bottom flask was equipped with an overhead stirrer, reflux condenser, thermocouple temperature read out, and heating mantle. The flask was purged with dry nitrogen and the following reaction conducted under an atmosphere of dry nitrogen. The flask was charged with 100 g of N-salicyloyl-10-aminodecanoic acid and 500 mL absolute ethanol. The slurry was heated to about 40° C. with stirring and all of the solids were dissolved. An addition funnel was attached to the reactor and charged with 232.5 g of 11.2 wt % sodium hydroxide dissolved in absolute ethanol. The sodium hydroxide solution was added to the stirred reaction mixture over a fifteen minute period. The reflux condenser was removed from the reactor and replaced with a distillation head and receiver. The reaction mixture was distilled at atmospheric pressure until about 395 g of distillate was collected. The reaction mixture had become a thick slurry during this distillation. The mixture was allowed to cool to room temperature. The thick mixture was transferred to a sintered glass funnel and the solids recovered by vacuum filtration. The ethanol wet cake was placed in a 45° C. vacuum oven and dried to constant weight at full vacuum. The dried material had a weight of about 124.6 g.

1. customA 1 L Pyrex glass, four-neck, round bottom flask was equipped with an overhead stirrer
2. temperaturereflux condenser
3. temperatureheating mantle
4. customThe flask was purged with dry nitrogen
5. customthe following reaction
6. dissolutionall of the solids were dissolved
7. customAn addition funnel was attached to the reactor
8. customThe reflux condenser was removed from the reactor
9. distillationThe reaction mixture was distilled at atmospheric pressure until about 395 g of distillate
10. customwas collected
11. distillationduring this distillation
12. temperatureto cool to room temperature
13. customThe thick mixture was transferred to a sintered glass funnel
14. filtrationthe solids recovered by vacuum filtration
15. customwas placed in a 45° C.
16. customdried to constant weight at full vacuum