Reaktion #574493

Reaktionsgleichung

M-TMI

melamine

→

M-TMI MELAMINE

Lösungsmittel

DMSO

DMSO

DMSO

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthermometer, reflux condenser, nitrogen inlet
2. 2
   TemperaturThe reaction temperature was maintained for an additional hour
3. 3
   TemperaturTo maintain efficient agitation
4. 4
   workup.ADDITIONthe thickening slurry was diluted several times
5. 5
   Filtrationthe reaction mixture was filtered
6. 6
   Waschenthe white solid was rinsed on
7. 7
   Filtrationa filter with THF (tetrahydrofuran)
8. 8
   Filtrationthe product was filtered
9. 9
   Waschenrinsed on the
10. 10
    Filtrationfilter with THF
11. 11
    Sonstigedried first in a hot air circulation oven at 60° C. overnight (16 hours)
12. 12
    workup.WAITin a vacuum oven (full pump vacuum) at 90°- 100° C. for 4 hours
13. 13
    WaschenFrom the first filtrate 85 g and from the second (wash) 73 g of white solids
14. 14
    Sonstigewere recovered

Vorschrift

In a 2 liter three neck glass reactor equipped with agitator, thermometer, reflux condenser, nitrogen inlet and dropping funnel, 252 g (2 moles) of melamine was dispersed in 800 ml of DMSO (Dimethylsulfoxide) under vigorous agitation. A solution of 423 g (2.1 moles) of M-TMI in 200 ml DMSO was added to the slurry at 110°-113° C. in 3.5 hours. The reaction temperature was maintained for an additional hour. To maintain efficient agitation, the thickening slurry was diluted several times during the reaction with a total of 150 ml of DMSO. After cooling to ambient temperature, the reaction mixture was filtered, the white solid was rinsed on a filter with THF (tetrahydrofuran) and reslurried in 800 ml of THF. After agitation at 64° C. for 80 minutes, the product was filtered, rinsed on the filter with THF and dried first in a hot air circulation oven at 60° C. overnight (16 hours), then in a vacuum oven (full pump vacuum) at 90°- 100° C. for 4 hours. The yield of the white solid product was 665 g. From the first filtrate 85 g and from the second (wash) 73 g of white solids were recovered. Infrared (IR) and Thermal Gravimetric Analysis (TGA) indicated that these products still contained 15-20% of DMSO.

Quelle