Method for quickly preparing cis-octahydropyrrolo[3,2-b]pyrrole
A technology of octahydropyrrole and 2-b, which is applied in the production of bulk chemicals, organic chemistry, etc., can solve the problems of harsh reaction conditions, inconvenient reaction operation, long reaction route, etc., achieve short reaction time, reasonable reaction process selection, Conducive to the effect of process amplification
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Embodiment 1
[0015] Compound 1 (10.0 g, 45.6 mmol), allyl bromide (7.9 g, 137 mmol), p-toluenesulfonic acid (11.8 g, 68.4 mmol) and anhydrous sodium sulfate (25.1 g) were added into xylene (200 mL) . The reaction mixture was heated to reflux and stirred for 20 hours. The reactant was cooled and filtered. After the filtrate was concentrated, Compound 2 (6.1 g) was obtained as a yellow oil with a yield of 53.2%.
[0016] To a solution of compound 2 (10.5 g, 40.6 mmol) in methanol (100 mL) was added ammonium acetate (31.2 g, 405 mmol). The reaction mixture was heated to reflux for 1 hour and then cooled to 30°C. Sodium cyanoborohydride (10.2 g, 162 mmol) was added in portions. The reaction mixture was heated to reflux for 1 hour. After the reaction was cooled, ice water (50 mL) was added to quench the reaction. Extracted with ethyl acetate (3x50 mL). The organic phase was extracted with 4N hydrochloric acid solution (3x50mL), the aqueous phase was washed with diethyl ether (100mL), sodi...
Embodiment 2
[0020] Compound 1 (10.0 g, 45.6 mmol), allyl chloride (7.9 g, 137 mmol), benzenesulfonic acid (11.8 g, 68.4 mmol) and anhydrous magnesium sulfate (25.1 g) were added to toluene (200 mL). The reaction mixture was heated to reflux and stirred for 20 hours. The reactant was cooled and filtered. After the filtrate was concentrated, Compound 2 (5.83 g) was obtained as a yellow oil with a yield of 50.2%.
[0021] To a solution of compound 2 (10.5 g, 40.6 mmol) in ethanol (100 mL) was added ammonium acetate (31.2 g, 405 mmol). The reaction mixture was heated to reflux for 1 hour and then cooled to 30°C. Sodium acetate borohydride (10.2 g, 162 mmol) was added portionwise. The reaction mixture was heated to reflux for 1 hour. After the reaction was cooled, ice water (50 mL) was added to quench the reaction. Extracted with ethyl acetate (3x50 mL). The organic phase was extracted with 4N hydrochloric acid solution (3x50mL), the aqueous phase was washed with diethyl ether (100mL), so...
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