Synthetic Route of 2862-39-7, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 2862-39-7 name is 2-Bromo-N,N-dimethylethanamine hydrobromide, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
General procedure: Example 54A 3-Ethyl-5-methyl-1-(2,2,2-trifluoroethyl)thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione 1.0 g (4.76 mmol) of the compound from Ex. 42A and 2.32 g (7.13 mmol) of caesium carbonate were stirred in 12 ml of anhydrous DMF at RT for 10 min, before 700 mul (7.13 mmol) of 1,1,1-trifluoro-2-iodoethane were added. Then the reaction mixture was heated in a microwave oven (Biotage Initiator with dynamic control of irradiation power) to 120 C. for 4 h. After cooling to RT, the mixture was diluted with ethyl acetate and washed successively with water and saturated sodium chloride solution. After drying over anhydrous magnesium sulphate, the mixture was filtered and concentrated to dryness. The residue obtained was purified by MPLC (Biotage cartridge, 100 g of silica gel, cyclohexane/ethyl acetate 3:1). After combination of the product fractions, concentration and drying under high vacuum, 592 mg (42% of theory) of the title compound were obtained. 1H-NMR (400 MHz, DMSO-d6, delta/ppm): 10.09 (s, 1H), 4.00 (t, 2H), 3.91 (q, 2H), 2.79 (s, 3H), 2.58 (t, 2H), 2.20 (s, 6H), 1.13 (t, 3H). LC/MS (Method 1, ESIpos): Rt=0.39 min, m/z=310 [M+H]+.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Bromo-N,N-dimethylethanamine hydrobromide, and friends who are interested can also refer to it.
Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; HAeRTER, Michael; KOSEMUND, Dirk; DELBECK, Martina; KALTHOF, Bernd; WASNAIRE, Pierre; SUessMEIER, Frank; LUSTIG, Klemens; (369 pag.)US2018/65981; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary