反应详情

温度

50 °C

A 22L, five neck round bottom flask, was equipped with an overhead stirrer, reflux condenser, thermocouple temperature read out, and heating mantle. The following reaction was run under a dry nitrogen atmosphere. Reagent acetone (13000 mL) and 4-[(4-chloro-2-hydroxy-benzoyl)amino]butanoic acid (500.0 g, 1.94 mol) were charged to the reactor and stirring was started. The reaction slurry was heated to 50° C. until a hazy brown solution was obtained. The warm solution was pumped through a warm pressure filter dressed with Whatman #1 paper into a clean 22 L reactor. The clear yellow filtrate was heated to 50° C. while stirring. Sodium hydroxide solution (50% aqueous; 155 g, 1.94 mol) was charged to the reactor while maintaining vigorous agitation. After the base addition was complete, the reactor was heated to reflux (60° C.) for 2.5 hours and then allowed to cool slowly to ambient temperature. The product was isolated by vacuum filtration through a sintered glass funnel and dried in a vacuum oven at 50° C. for 24 hours to give 527.3 g of sodium 4-[(4-chloro-2-hydroxybenzoyl)amino]butanoate as an off-white solid. Using acetone in the final stage of the synthesis always resulted in the production of the anhydrous crystalline form. The yield was 97.2%.

1. temperaturereflux condenser
2. temperatureheating mantle
3. customThe following reaction
4. customwas obtained
5. filtrationfilter
6. customdressed with Whatman #1 paper into a clean 22 L reactor
7. temperatureThe clear yellow filtrate was heated to 50° C.
8. stirringwhile stirring
9. temperaturewhile maintaining vigorous agitation
10. additionAfter the base addition
11. temperaturethe reactor was heated
12. temperatureto reflux (60° C.) for 2.5 hours
13. temperatureto cool slowly to ambient temperature
14. customThe product was isolated by vacuum filtration through a sintered glass funnel
15. customdried in a vacuum oven at 50° C. for 24 hours