Process for production of optically active amine derivatives
A technology of ethylamine and reaction product, applied in the field of optically active amine derivatives, can solve the problems of generating dimers and the like that are not described
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reference example 1
[0112] 2,3-Dihydrobenzofuran-5-carbaldehyde (carbaldehyde)
[0113]
[0114]Mix and heat 2,3-dihydrobenzofuran (100g, 832mmol) and N,N-dimethylformamide (134g, 1830mmol), and add three Phosphorus oxychloride (255 g, 1643 mmol). The reaction mixture was heated at an internal temperature of 80-90°C and stirred for 7.5 hours. The resulting mixture was then added dropwise to water (1000 g) under cooling, and stirred at room temperature for 5 hours. The resulting mixture was extracted with toluene, the extract was washed sequentially with water, saturated aqueous sodium bicarbonate and water, and the organic layer was concentrated in vacuo to obtain a toluene solution of the title compound (yield 340 g, apparent yield 100%).
reference example 2
[0116] (E)-3-(2,3-dihydrobenzofuran-5-yl)ethyl acrylate
[0117]
[0118] Under cooling, triethyl phosphonoacetate (205 g, 916 mmol) was added dropwise to a solution (340 g) of 2,3-dihydrobenzofuran-5-carbaldehyde (832 mmol) in toluene obtained in the above step . Then a suspension of sodium tert-butoxide (sodium t-butylae) (88.0g, 1187mmol) in toluene (530g) was added dropwise, stirred for 1 hour, and then acetic acid (20g) and water (500g) were added dropwise ). The reaction mixture was warmed to room temperature and the layers were separated. The organic layer was washed sequentially with saturated aqueous sodium bicarbonate and water, and the organic layer was concentrated under vacuum to less than 300 mL. Methanol (396 g) was then added to the residue and heated and dissolved. To this solution was added water (500 g) dropwise at room temperature, and stirred to precipitate crystals, which were collected by filtration and dried under reduced pressure to obtain the t...
reference example 3
[0120] 3-(2,3-Dihydrobenzofuran-5-yl) ethyl propionate
[0121]
[0122] (E)-Ethyl 3-(2,3-dihydrobenzofuran-5-yl)acrylate (50.0 g, 227 mmol) was dissolved in acetic acid (312 g), and the reaction system was replaced with nitrogen. Then, 5% Pd / C (4.96 g, dry weight) was added to the solution and pressurized to 196-294 KPa with hydrogen. Under the pressure of 196~294KPa, at 50 ℃, the mixture was reacted for 1 hour, the catalyst was filtered and washed with acetic acid (208g) to obtain an acetic acid solution of the title compound (yield 569g, apparent yield 100%).
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