Method for preparing 5-(tert-butoxycarbonyl)-2-oxooctahydropyrrolo[3, 4-b]pyrrole-3a-carboxylic acid
A kind of technology of oxyethylene octahydropyrrole and tert-butoxycarbonyl, which is applied to the preparation method of 5-tert-butoxycarbonyl-2-oxygenide octahydropyrrolo[3,4-b]pyrrole-3a-carboxylic acid It can solve the problems such as the lack of suitable industrial synthesis methods, and achieve the effects of reasonable reaction process design, easy reaction and cost saving.
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[0012] Compound 1 (100 g, 38.9 mmol), ethyl bromoacetate (130 g, 0.78 mol) and tetrabutylammonium fluoride (122 g, 0.47 mol) were dissolved in 1500 mL tetrahydrofuran at 25°C, and stirred at 25°C for 12 Hours, after the reaction was over, the reaction solution was spin-dried, and the obtained crude product was dissolved in 3000 mL of ethyl acetate, washed three times with water, dried and spin-dried, and column chromatography obtained 74 g of compound 2 as a yellow oil, yield: 56%. H NMR: CDCl3 400MHz δ 1.22-1.29 (m, 6H), 1.5 (s, 9 H), 2.96-3.08 (m 1H), 3.57-3.60 (m, 1H), 3.91-4.00 (m, 2H), 4.08-4.32 (m, 6H).
[0013] Compound 2 (30 g, 87.4 mmol), hydroxylamine hydrochloride (9.1 g, 131.1 mmol) and sodium bicarbonate (11 g, 131.1 mmol) were dissolved in a mixed solvent of 150 ml tetrahydrofuran and 300 mL ethanol, and stirred at 25 °C for 12 Hour. After the reaction, ethanol and tetrahydrofuran were spin-dried, and the obtained crude product was dissolved in 1000 mL of ethyl...
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