反应详情

温度

50 °C

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