Adding a certain compound to certain chemical reactions, such as: 5003-71-4, name is 3-Bromopropan-1-amine hydrobromide, belongs to bromides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 5003-71-4, COA of Formula: C3H9Br2N
To a mixture of 3-bromopropan-1 -amine hydrobromide (98.5 g, 45 mmol, 1 .0 eq) and Boc20 (93.3 g, 42.8 mmol, 0.95 eq) in DCM (500 ml) was added dropwise DIPEA (64.0 g, 49.5 mmol). The resulting mixture was stirred at room temperature overnight. Then, the reaction mixture was washed with water, 1 N HCI and brine, dried over Na2S04 and filtered. The solvent was evaporated to give the expected compound (95.8 g, 94% yield) as a white solid.To a suspension of NaH (60 % in mineral oil) (1 1.1 g, 278 mmol, 1 .3 eq) in DMF (150 ml) was added dropwise a solution of 2-(1 H-indol-3-yl)acetamide (37.2 g, 214 mmol, 1 .0 eq) in DMF (150 ml) at 0C under N2 and the reaction mixture was stirred for 30 min. Then a solution of the previous compound (55.9 g, 235 mmol, 1.1 eq) in DMF (100 ml) was added dropwise at 0 C. The mixture was stirred at 0 C for 30 min and at room temperature for 10 hrs. The reaction mixture was diluted in water (500 ml) and extracted with ethyl acetate. The organic phase was washed with brine, dried over Na2S04 and filtered. The solvent was evaporated under vacuum. The crude product was purified by column chromatography over silica gel eluted with MeOH/DCM (0/100 to 3/97) to give the intermediate 3 (52.8 g, 75% yield) as a solid.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Bromopropan-1-amine hydrobromide, and friends who are interested can also refer to it.
Reference:
Patent; AMAKEM NV; LEYSEN, Dirk; DEFERT, Olivier; BOLAND, Sandro; WO2013/4709; (2013); A1;,
Bromide – Wikipedia,
bromide – Wiktionary