Piperazine compound and preparation and usage thereof
A compound and pharmaceutical technology, applied in the field of medicine, can solve problems such as hypoglycemia, weight gain, and inability to maintain long-term curative effect, and achieve the effect of lowering blood sugar inhibition and lowering blood sugar significantly
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Embodiment 1
[0058] 1-(6,7-Dihydrothieno[3,2-c]pyridin-5(4H)-yl)-2-(4-(tetrahydrofuran-2-carbonyl)piperazin-1-yl)ethanone
[0059]
[0060] Add 21.5g of intermediate II-1 to the reaction flask equipped with stirring, condenser and thermometer, dissolve it with 80ml of acetonitrile and 20.2g of triethylamine, then add piperazin-1-yl (tetrahydrofuran-2-yl) 18.4 g of methyl ketone was stirred at room temperature for 7 hours, the reaction solution was washed with saturated brine (50ml×3), the organic layer was dried over anhydrous sodium sulfate, filtered, and the organic solvent was rotary evaporated, and the residue was separated by silica gel column chromatography to obtain Yellow liquid (HPLC: 99.5%). HRMS(m / z)[M+H] + : 364.1682. 1 H-NMR (400MHz, DMSO-d6) δ: 1.773-1.841 (m, 2H), 1.935-2.013 (m, 2H), 2.380-2.425 (t, 3H), 2.486-2.495 (t, 4H), 2.749 ( s, 1H), 2.886(s, 1H), 3.252-3.293(t, 2H), 3.432-3.488(m, 4H), 3.699-3.803(m, 4H), 4.505(s, 1H), 4.590-4.638( q, 2H), 6.876-6.888 (s, 1H)...
Embodiment 2
[0065] Compound I-1 into hydrochloride: Take 4.0 g of the yellow liquid product of I-1 and dissolve it in 11 mL of anhydrous ether. Cool in an ice-water bath to 5°C, add 11.1% diethyl ether solution of hydrochloric acid dropwise until the pH is 2, and continue stirring for about 1 h in an ice-water bath. Filter to obtain a light yellow solid.
Embodiment 3
[0067] Sulfate formation of compound I-2: Take 4.3 g of the yellow liquid product of I-2 and dissolve it in 25 mL of acetone. Cool in an ice-water bath to 5°C, add 9.8% sulfuric acid acetone solution dropwise until the pH is 3, and continue stirring for about 1 h in an ice-water bath. Filter to obtain a yellow solid.
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