反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
To 100 g of 1-bromo-3,5-dimethyl adamantane and 10 g of urea, adding 60 ml of anhydrous formic acid, heating to 150° C. and hold for 1 hour. Cooling to the room temperature and adding 95 ml of concentrated hydrochloric acid to hydrolyze at 100° C. for 1 hour. Adjusting with 30% sodium hydroxide solution until the solution becomes basic. Extracting with toluene twice, combining the organic layers and washing with water. Concentrating under reduced pressure to yield a limpid yellow solution as 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 acetone to yield 61.7 g of pure Memantine Hydrochloride. The yield is 69.5% (GC 99.9%).
WORKUP
后处理
- temperatureCooling to the room temperature
- waitto hydrolyze at 100° C. for 1 hour
- extractionExtracting with toluene twice
- washwashing with water
- concentrationConcentrating under reduced pressure