Aza (oxa)-cyclopentane-2- ketone (thione) compounds, medicine compositions thereof, preparation method and applications
A compound and cycloalkyl technology, applied in the field of pharmacy, can solve problems such as drug resistance, many side effects, and ineffective hypoglycemic effect
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Embodiment 1
[0090] Example 1: Preparation of important intermediate (S)-4(3,4-dimethoxybenzyl)oxazolidin-2-one
[0091]
[0092] Weigh levodopa 1a (purchased from Anaiji Chemical, 5.00g, 25.3mmol) and dissolve it in dioxane / water (50%, 80ml), add triethylamine (4.24ml, 30.4mmol), 0°C Di-tert-butyl dicarboxylate (6.64g, 30.4mmol) was added in batches, the reaction solution was stirred at this temperature for half an hour, and stirred at room temperature for 18h. After TLC detected that the reaction was complete, the solvent was vacuum-dried, and 30ml of water and 30ml of Ethyl acetate, acidified with 2M hydrochloric acid to pH = 1, separated, and extracted three times with ethyl acetate (20ml), combined organic phases, washed with saturated brine (3×20ml), dried over anhydrous sodium sulfate, filtered, vacuum The solvent was drained to give the crude product 2a. The crude product 2a was dissolved in acetone (50ml), potassium carbonate (12.25g, 88.0mmol) and dimethyl sulfate (8.15ml, 86...
Embodiment 2
[0095] Example 2: Preparation of (S)-4(3,4-dimethoxybenzyl)-3(3-methoxybenzyl)oxazolidin-2-one (yhhu3000)
[0096]
[0097] Weigh 5a (100mg, 0.42mmol) in a 10ml round bottom flask, add 3ml THF, slowly add 60% sodium hydride (34mg, 0.84mmol), add m-methoxybenzyl bromide (with m-methoxybenzaldehyde and boron Sodium hydride was reacted to obtain methoxybenzyl alcohol, which was then reacted with phosphorus tribromide, the same below) (93mg, 0.46mmol), reacted at room temperature overnight, and TLC detected that the reaction was complete, adding 3ml of water to extract it, and ethyl acetate ( 3×10ml) extraction, combined organic phases, dried over anhydrous sodium sulfate, dried the solvent under reduced pressure, column chromatography (petroleum ether / ethyl acetate=2:1), and obtained the target (S)-4(3,4 -dimethoxybenzyl)-3(3-methoxybenzyl)oxazolidin-2-one (112 mg, 75%). 1 H NMR (300MHz, CDCl 3 )δ7.25(dd,J=9.0,6.7Hz,1H),6.85-6.70(m,4H),6.60(d,J=8.1Hz,1H),6.49(s,1H),4.79(d,J ...
Embodiment 3
[0098] Example 3: Preparation of (S)-4(3,4-dimethoxybenzyl)-3(3-benzyloxybenzyl)oxazolidin-2-one (yhhu3001)
[0099]
[0100] In addition to replacing m-methoxybenzyl bromide with 3-benzyloxybenzyl bromide, compound (S)-4(3,4-dimethoxybenzyl)-3 was obtained according to a method similar to that shown in Example 2 (3-Benzyloxybenzyl)oxazolidin-2-one. 1 H NMR (300MHz, CDCl3) δ7.50–7.25(m,5H),6.93(d,J=8.5Hz,1H),6.90–6.80(m,2H),6.77(d,J=8.1Hz,1H) ,6.59(d,J=8.1Hz,1H),6.48(s,1H),5.05(s,2H),4.80(d,J=15.2Hz,1H),4.16-3.95(m,3H),3.84( s, 3H), 3.78 (s, 3H), 3.80–3.70 (m, 1H), 2.98 (dd, J=13.7, 5.0Hz, 1H), 2.55 (dd, J=13.9, 8.5Hz, 1H).
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