Réaction #986755

Équation de réaction

1-bromo-3,5-dimethyl adamantane

urea

hydrochloric acid

→

1-amino-3,5-dimethyl adamantane

Solvants

formic acid

Conditions de réaction

Traitement

1. 1
   TempératureCooling to the room temperature
2. 2
   workup.WAITto hydrolyze at 80° C. for about 1 hour
3. 3
   ExtractionAdjusting with 30% sodium hydroxide to a pH of 12, extracting with toluene twice
4. 4
   Lavagewashing with water
5. 5
   ConcentrationConcentrating under reduced pressure

Mode opératoire

To 100 g of 1-bromo-3,5-dimethyl adamantane and 86 g of urea, adding 80 ml of 80 wt % formic acid, heating to 80° C. and holding for 3 hours. Cooling to the room temperature and adding 95 ml of concentrated hydrochloric acid to hydrolyze at 80° C. for about 1 hour. Adjusting with 30% sodium hydroxide to a pH of 12, extracting with toluene twice, combining the organic layers and washing with water. Concentrating under reduced pressure to yield a limpid yellow solution as the 1-amino-3,5-dimethyl adamantane crude. To the crude, adding 150 ml of ethanol and concentrated hydrochloric acid, heating to dissolve and crystallizing to yield white solid. Drying the solid and re-crystallizing with ethanol to yield 61.0 g of pure Memantine Hydrochloride. The yield of product is 68.8% (GC 99.5%).

Source