Reaktionsgleichung
[N+:1]([CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)([O-:3])=[O:2].[CH2:11]=[O:12].O.[C:14](=[O:17])([O-])[O-].[Na+].[Na+]>>[N+:1]([C:4]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)([CH2:14][OH:17])[CH2:11][OH:12])([O-:3])=[O:2]Komponenten
Reaktionsbedingungen
- Temperatur
- 38 °C
Versuchsvorschrift
100 g. (0.73 mole) of nitromethylbenzene, 131.5 g. (1.61 mole) of 37% formaldehyde and 1.8 g. of sodium carbonate monohydrate are placed in a 500 ml. beaker equipped with a mechanical stirrer. The mixture is stirred, the temperature rises to 38° C. and is maintained at 38° C. by using a cold water bath. After 11/2 hours, crystals begin to form. The mixture is diluted with 210 ml. of ice water and stirred at 10° C. for about 2 hours. The mixture is filtered and the filtrate washed with water. The damp cake is placed back in the beaker and 280 ml. of ice water is added. The mixture is stirred for 1 hour, filtered and air dried overnight. The solid is stirred with 250 ml. of toluene for about 1 hour at 10° C. and filtered, then washed with cold toluene and dried. The yield is 112.6 g. of nitrophenyldiol (78%), M.P. 96°-97.5° C.
Aufarbeitung
- custombeaker equipped with a mechanical stirrer
- customrises to 38° C.
- custom2 hours, crystals
- customto form
- additionThe mixture is diluted with 210 ml
- filtrationThe mixture is filtered
- washthe filtrate washed with water
- additionof ice water is added
- stirringThe mixture is stirred for 1 hour
- filtrationfiltered
- customair dried overnight
- stirringThe solid is stirred with 250 ml
- filtrationfiltered
- washwashed with cold toluene
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-b2bae14414914d758e9589d6697ea9c9
- Quelldatensatz
- uspto-grants-1989_09
- Patentnummer
- US04868327
Verknüpfte Notizen
Wird geladen…