Reference of 941-37-7, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 941-37-7 as follows.
To 100g of 1-bromo-3, 5-dimethyl adamantane and 86g of urea, adding 80ml of 80wt% formic acid, heating to 80C and holding for 3 hours. Cooling to the room temperature and adding 75ml of 85% phosphoric acid to hydrolyze at 80C for 1 hour. Adjusting with 10% potassium hydroxide aqueous solution 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 1-amino-3,5-dimethyl adamantane crude. To the crude, adding 150ml of ethanol and concentrated hydrochloric acid, heating to dissolve and crystallizing to yield a white solid. Drying the solid and re-crystallizing with ethanol to yield 61.0g of pure Memantine Hydrochloride. The yield is 68.8% (GC 99.5%). 1HNMR (CDCl3, 400MHZ): delta0.833 (6H, singlet), 1.156 (2H, quartet), 1.328 (4H, quartet), 1.683(4H, quartet), 1.869 (2H, broad signal), 2.179 (1H, broad signal), 8.28 (3H, broad signal). MS (Q-Tof micro, ESI+): 179(M+), 164, 122, 108, 93 and 55. Element Analysis (C12H21N.HCl): actual results (calculated value%): C 66.77 (66.80), H 10.40 (10.28), N 6.48(6.49) and Cl 16.39(16.43)
According to the analysis of related databases, 941-37-7, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Shanghai Institute of Pharmaceutical Industry; Zhejiang Kangyu Pharmaceutical Co., Ltd.; EP1674446; (2006); A1;,
Bromide – Wikipedia,
bromide – Wiktionary