Reaktion #89599

Reaktionsgleichung

sodium hydroxide

methacryloyl chloride

methacryloyl chloride

methacryloyl chloride

chloric acid

1-aminobenzene-3,4,5-tricarboxylic acid

sodium hydroxide

→

Benzene Tricarboxylic Acid

Lösungsmittel

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeA 2 litter flask equipped with a magnetic stirrer
2. 2
   workup.DISSOLUTIONWhen this was dissolved
3. 3
   workup.DISSOLUTIONdissolved
4. 4
   TemperaturAfter neutralization heat
5. 5
   Sonstigethe reaction result
6. 6
   TemperaturWhile this was maintained below 15° C.
7. 7
   workup.ADDITIONThis solution was added to the reaction mixture 20 minutes
8. 8
   TemperaturAfter the reaction product was cooled down to 10° C.
9. 9
   Temperaturwas maintained below 15° C
10. 10
    Sonstige20 minutes
11. 11
    ExtraktionThe thus-produced solid portion was extracted by vacuum filtration
12. 12
    Waschenby washing with ethanol
13. 13
    Sonstigedried at 60° C. for 14 hours in a vacuum oven

Vorschrift

A 2 litter flask equipped with a magnetic stirrer, a thermometer, and 250 ml dripping funnel were filled with 1 litter of water and 71 g of sodium hydroxide pellet. When this was dissolved, 100 g of 1-aminobenzene-3,4,5-tricarboxylic acid was added and dissolved. After neutralization heat ceased, the reaction result was cooled down to 10° C. The dripping funnel was filled with 40.23 g of methacryloyl chloride. While this was maintained below 15° C., the liquid was dripped to the reaction container in 15 minutes. 40 g of sodium hydroxide was dissolved in 150 g of water in another container. This solution was added to the reaction mixture 20 minutes after the addition of methacryloyl chloride was complete. After the reaction product was cooled down to 10° C., 40 g of methacryloyl chloride was dripped from the dripping funnel in 15 minutes while the temperature was maintained below 15° C. 20 minutes after the dripping was complete, the reaction mixture was acidized to pH 3 by strong chloric acid. The thus-produced solid portion was extracted by vacuum filtration followed by washing with ethanol and dried at 60° C. for 14 hours in a vacuum oven.

Quelle