Synthetic Route of 78531-29-0,Some common heterocyclic compound, 78531-29-0, name is 1,3-Dimethoxypropan-2-amine, molecular formula is C5H13NO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Intermediate 222: (4-((1,3-Dimethoxypropan-2-yl)amino)-3-nitrophenyl)methanol To a solution of (4-fluoro-3-nitrophenyl)methanol (16 g, 93 mmol) in THF (80 mL) was added 1,3- dimethoxypropan-2-amine (10 g, 84 mmol) and DIPEA (15 mL, 86 mmol). The mixture was split into seven portions and heated under microwave conditions at 100 C for 7 hours. The reaction mixture was partitioned between ethyl acetate (3 x 500 mL) and saturated aqueous sodium bicarbonate solution (750 mL). The organic layers were combined, washed with saturated brine (500 mL), and evaporated under reduced pressure. The sample was loaded in dichloromethane and purified SPE (silica, 100 g) using a gradient of 0-80% EtOAc in cyclohexane. The appropriate fractions were combined and evaporated under reduced pressure to give a the title compound (12.0 g, 44.4 mmol). LCMS (System B): tRET = 0.85 min, MH+ = 271. Less pure fractions were combined and evaporated. The sample was loaded in dichloromethane and purified by SPE (silica, 100 g) using a gradient of 0- 50 % EtOAc in cyclohexane. The appropriate fractions were combined and evaporated under reduced pressure to give the title compound (3.7 g, 13.69 mmol). LCMS (System J): tRET = 0.85 min, MH+ = 271.
The synthetic route of 78531-29-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; BIT, Rino Antonio; BROWN, John Alexander; HUMPHREYS, Philip G.; JONES, Katherine Louise; (240 pag.)WO2016/146738; (2016); A1;,
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