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. 5003-71-4, name is 3-Bromopropan-1-amine hydrobromide, A new synthetic method of this compound is introduced below., category: bromides-buliding-blocks
Example 1 Preparation of Tert-Butyl 3-Bromopropylcarbamate To a solution of sodium hydroxide (105 g, 2.625 mol) in water (1.15 L) maintained at a temperature at or slightly below 10 C. was added a solution of di-tert-butyl dicarbonate (229 g, 1.05 mol) in heptane (1.03 L). The flask containing the solution of di-tert-butyl dicarbonate was rinsed with heptane (125 mL) and the rinsate was added to the reaction mixture. The resulting mixture was cooled to a temperature at or slightly below 10 C. and a solution of 3-bromopropylamine hydrobromide (251 g, 1.15 mol) in water (250 mL) was added dropwise at a rate that allowed the internal reaction temperature to be maintained below about 20 C. The flask containing the solution of 3-bromopropylamine hydrobromide was rinsed with water (20 mL) and the rinsate was added to the reaction mixture. After the addition was complete, the reaction mixture was allowed to slowly warm to room temperature (about 22 C.) and stirring was continued for about 2 hours at room temperature. The stirring was discontinued and the mixture was allowed to stand for 30 minutes. The lower aqueous layer was separated from the organic layer and discarded. To the organic layer was added a saturated aqueous sodium chloride solution (250 mL) and the resulting mixture was stirred for 5 min. The mixture was allowed to stand for 30 minutes and the lower aqueous layer was separated and discarded. The organic layer was concentrated to a volume of about 350 mL and this concentrated solution was cooled to 5 C. and stirred for 4 hours at 5 C. The resulting precipitate was collected by vacuum filtration to provide the title compound as a white crystalline solid (211 g, 84% yield). The filtrate was concentrated and the concentrated solution was cooled to 5 C. and stirred for 4 hours at 5 C. The resulting additional precipitate was collected by vacuum filtration to provide an additional amount of the title compound (17 g, 6.8% yield). 1H NMR (400 MHz, DMSO-d6) delta 1H NMR (400 MHz, DMSO-d6) delta 3.50 (t, J=6.8 Hz, 2H), 3.03 (q, J=6.8 Hz, 2H), 1.91 (m, J=6.8 Hz, 2H), 1.38 (s, 9H).
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; THERAVANCE, INC.; Zhang, Weijiang; Tracey, Michael R.; Lee, Junning; US2014/275554; (2014); A1;,
Bromide – Wikipedia,
bromide – Wiktionary