The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 53398-55-3, name is 1-Bromo-3,5,7-trimethyladamantane, A new synthetic method of this compound is introduced below., HPLC of Formula: C13H21Br
Example 6: l-Acetamido-3.5.7-dirnethyladamantane (Ac-NH-TMAD) synthesis; 4 g of l-bromo-3,5,7-trimethyladamantane, 12 g (15 ml) of acetonitrile, and 7 g of 75% phosphoric acid are added to a 50ml reactor equipped with condenser, mechanical stirrer, thermometer at 20-250C and under nitrogen. After addition, the internal temperature rises to 30-320C. The obtained biphasic system is warmed to 87+/-2C over about 30 min (slight reflux) and the temperature maintained for 17 hrs. During the course of the reaction, a monophasic system is obtained. At this point, the reaction is complete. n-butanol (15ml), toluene (15ml) and water (15ml) are added and the resulting biphasic system is cooled to 20-250C. Sodium hydroxide 30% is added to reach pH 6-7 and the temperature rises to 40-450C. Phases are separated at 35-400C and the aqueousphase is discarded. Water (15ml) is loaded to the organic phase and, after stirring and standing, the phases are separated at 40-45. The organic phase is concentrated under vacuum (res. pressure 45-50 mmHg, external temperature 80-850C, internal temperature 40-700C) until a residual volume of 6-6.5ml is obtained. After cooling to 55-600C, acetone (30ml) is added. The resulting suspension is warmed to reflux (62-63C) until complete dissolution is obtained. After cooling to 500C, water (50ml) is slowly added and crystallization of l-acetamido-3,5,7-dimethyladamantane occurs. After 1.5-2hrs at 18+/-3C, the solid is filtered, washed with water and dried at 45-500C for 15hrs. Dry weight: 3.3g 1H NMR is reported: 1H-NMR in CDCl3 (298K)
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; TEVA PHARMACEUTICAL FINE CHEMICALS S.R.L.; TEVA PHARMACEUTICALS USA, INC.; WO2007/126886; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary