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. 2862-39-7, name is 2-Bromo-N,N-dimethylethanamine hydrobromide, A new synthetic method of this compound is introduced below., Product Details of 2862-39-7
60% NaH (0.215 g, 5.39 mmol) was suspended in DMF (4 ml) and the suspension was stirred at room temperature under nitrogen. A solution of N-(3-allyl-4-hydroxyphenyl)acetamide (1 .03 g, 5.39 mmol) in DMF (5 ml) was added and the brown mixture was stirred for 15 min. 2-bromo- Nu,Nu-dimethylethanamine, hydrobromide (0.627 g, 2.69mmol) was added as a solid and the mixture was stirred at room temperature for 48h. Additional 60% NaH (0.215 g, 5.39 mmol) was added followed by addition of 2-bromo-N,N-dimethylethanamine, hydrobromide (0.627 g, 2.69mmol) and the reaction was stirred for 18h at room temperature. Added an additional 1 .0 eq of NaH (215 mg) and stirred 1 hour at room temperature. The reaction was poured into ice- water and stirred until the ice had melted. The solution was transferred to a separatory funnel and the pH was adjusted to 8 using 2M HCI. The solution was extracted with ether and the ether was washed with 2M NaOH, water, dried over sodium epsilonmubetabeta, filtered, and concentrated. The GammaThetaepsilonmuIota-Gamma^ solid was purified via silica gel chromatography (Biotage Isolera, 24 g column, 0-15% MeOH:DCM over 45 min, loaded as a solution in DCM) to give the desired product (88.0 mg, 6%) as a pale yellow solid. LC-MS (ES) m/z = 263.2 [M+H]+ NMR (400 MHz, DMSO-d6) delta ppm 1 .99 (s, 3 H) 2.22 (s, 6 H) 2.62 (t, J=5.75 Hz, 2 H) 3.28 (d, J=6.85 Hz, 2 H) 4.01 (t, J=5.87 Hz, 2 H) 4.97 – 5.10 (m, 2 H) 5.92 (ddt, J=16.93, 10.09, 6.79, 6.79 Hz, 1 H) 6.89 (d, J=8.80 Hz, 1 H) 7.28 (d, J=2.45 Hz, 1 H) 7.40 (dd, J=8.80, 2.69 Hz, 1 H) 9.71 (s, 1 H).
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; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; DUFFY, Kevin J.; PARRISH, Cynthia Ann; ATOR, Laura E.; BASKARAN, Subramanian; DARCY, Michael Gerard; OPLINGER, Jeffrey Alan; RALPH, Jeffrey M.; RIDGERS, Lance Howard; TIAN, Xinrong; ZHANG, Cunyu; (225 pag.)WO2019/53617; (2019); A1;,
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