Compound of new benzo heterocycle categories, preparation method and application
A technology of compounds and heterocycles is applied in the preparation of anti-type II diabetes drugs and the synthesis of benzoheterocycles, and can solve problems such as liver toxicity and weight gain.
Patent Information
- Authority / Receiving Office
- CN · China
- Current Assignee / Owner
- Publication Date
- 2007-12-26
- Estimated Expiration
- Not applicable · inactive patent
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Abstract
Description
technical field
[0001] The invention relates to the fields of medicinal chemistry and endocrine therapy, in particular to the synthesis of benzoheterocyclic compounds and their use in the preparation of anti-II diabetes drugs. Background technique
[0002] Diabetes mellitus is a group of clinical syndromes characterized by chronic hyperglycemia (fasting blood glucose concentration greater than 130 mg / dL) and glucosuria due to abnormal carbohydrate, fat and protein metabolism caused by insufficient insulin secretion or insulin resistance. Sustained hyperglycemia can lead to many complications, such as retinal, renal, nervous system lesions and vascular complications, especially cardiovascular complications are the main threat to death and disability in diabetic patients, so controlling the patient's blood sugar level is very important for delaying or preventing diabetes. Interruption complications are extremely important. The traditional antidiabetic drugs mainly include big...
Examples
Embodiment 1
[0126] Example 1: 6-(2-(5-methyl-2-phenyl-4-oxazole)ethoxy)-4-oxo-4H-benzopyrone-2-carboxylic acid methyl ester Preparation (compound 1)
[0127]2-(5-methyl-2-phenyl-4-oxazole) ethanol 0.14g (0.69mmol), 6-hydroxy-4-oxo-4H-benzopyrone-2-carboxylic acid methyl ester 0.15 g (0.69 mmol) was dissolved in 20 ml of anhydrous tetrahydrofuran, 0.21 g (0.79 mmol) of triphenylphosphine was added, and 0.16 ml (0.79 mmol) of diisopropyl azodicarboxylate was added dropwise at 0°C. Stir at room temperature for 12 hours. The solvent was distilled off under reduced pressure, and the residue was dissolved in methanol to precipitate a white solid. The resulting solid was recrystallized from methanol to obtain 0.22 g of the target product, yield: 79.7%. M.P. 154-155°C. 1 HNMR (CDCl 3 ): δ=2.39(s, 3H), 3.02(t, J=6.59Hz, 2H), 4.00(s, 3H), 4.35(t, J=6.59Hz, 2H), 7.09(s, 1H), 7.32 (dd, J=9.20Hz, J=3.16Hz, 1H), 7.43(m, 3H), 7.53(d, J=9.02Hz, 1H), 7.56(d, J=3.02Hz, 1H), 7.98(dd , J=8.10Hz, J=2.0...
Embodiment 2
[0130] Embodiment 2: the preparation of 6-(2-(5-methyl-2-phenyl-4-oxazole) ethoxy)-4-oxo-4H-benzopyrone-2-carboxylic acid ( Compound 2)
[0131] Compound 1 0.12 (0.30 mmol) prepared in Example 1 was dissolved in 15 ml of methanol, 1.5 ml of 2N NaOH solution was added, and the reaction was stirred at 45° C. for 1.5 hours. Evaporate the methanol solvent under reduced pressure, add water, adjust the pH value to about 2 with 10% hydrochloric acid, extract with 2×10ml ethyl acetate, wash the organic phase with water, wash with saturated brine, dry over anhydrous sodium sulfate, and evaporate the solvent under reduced pressure. The residue was recrystallized from methanol and ether to obtain 0.10 g of the product, yield: 86.3%. M.P.>200°C (oxidation). 1 H NMR (CDCl 3 ): δ=2.36(s, 3H), 2.98(t, J=6.58Hz, 2H), 4.35(t, J=6.58Hz, 2H), 7.03(s, 1H), 7.32(dd, J=9.20Hz , J=3.16Hz, 1H), 7.43(m, 3H), 7.53(d, J=9.02Hz, 1H), 7.56(d, J=3.02Hz, 1H), 7.98(dd, J=8.10Hz, J =2.06Hz, 2H). EI-MS (m...
Embodiment 3
[0134] Example 3: 6-(2-(5-methyl-2-(3-methyl)phenyl-4-oxazole)ethoxy)-4-oxo-4H-benzopyrone-2 - Preparation of methyl carboxylate (compound 3)
[0135] With 2-(5-methyl-2-(3-methyl)phenyl-4-oxazole)ethanol and 6-hydroxy-4-oxo-4H-benzopyrone-2-carboxylic acid methyl ester As the starting material, Compound 3 was prepared in the same manner as in Example 1, with a yield of 82.0%. M.P. 162-163°C. 1 H NMR (CDCl 3 ): δ=2.38(s, 3H), 2.40(s, 3H), 3.02(t, J=6.56Hz, 2H), 4.00(s, 3H), 4.34(t, J=6.56Hz, 2H), 7.09 (s, 1H), 7.22(d, J=7.63Hz, J=3.16Hz, 1H), 7.32(m, 2H), 7.53(d, J=9.15Hz, 1H), 7.56(d, J=3.05 Hz, 1H), 7.77 (d, J=7.76Hz, 1H), 7.82 (s, 1H). EI-MS (m / z): 4 1 9 (76, M + ), 200(100).
[0136] Elemental Analysis, C 24 h 21 NO 6 (419): Calculated C, 68.73; H, 5.05; N, 3.34.
[0137] Found values C, 68.50; H, 4.90; N, 3.25.