Selenourea derivatives, pharmaceutical compositions and uses thereof
The technology of a composition and a medicine is applied in the field of preparing the selenourea derivatives, and can solve the problems of unsatisfactory curative effect, drug resistance and the like
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Embodiment 1
[0149] Example 1: N-methyl-2-bis(pyridin-2 base)methyleneamino-selenourea
[0150] Step 1. S-Methylthio 4-methyl-3-thiosemicarbazide
[0151] Add 0.423g (4mmol) 4-methyl-3-thiosemicarbazide, 10ml absolute ethanol and 0.568g (4mmol) methyl iodide to a 50ml single-necked bottle, and react under reflux at 85°C for one hour to obtain S-methylthio 4 -The ethanol solution of methyl-3-thiosemicarbazide was cooled, solids were precipitated, and the solvent was spin-dried to obtain S-methylthio-4-methyl-3-thiosemicarbazide as a solid (0.43g, 90%).
[0152] Step 2. 4-Methyl-3-selenocarbazide
[0153] Add 0.42g (4mmol) of sodium carbonate to the newly prepared sodium selenate 0.41g (4mmol) ethanol (10ml) solution, and add 0.54g (4mmol) of S-methylthio 4-methyl-3-thiosemicarbazide ) solid was added to the ethanol solution of sodium hydrogen selenate, and reacted at room temperature for 20h to generate 4-methyl-3-selenacarbazide (0.49g, 80%).
[0154] After the reaction is completed, ad...
Embodiment 2
[0157] Example 2: 2-bis(pyridin-2 base)methyleneamino-selenourea
[0158] Method is with embodiment 1, intermediate selenaminocarbazide, 1 H-NMR (400MHz, DMSO) δppm: 4.521 (s, 2H), 7.644 (m, 1H), 7.985 (m, 1H), 9.082 (d, 1H), the product is yellow solid 2-di(pyridin-2yl) Methyleneamino-selenourea 1 H-NMR (400MHz, DMSO) δppm: 7.477-7.495 (m, 1H), 7.523-7.543 (d, 1H), 7.606-7.625 (m, 1H), 7.933-7.957 (m, 1H), 7.990-8.013 ( m, 1H), 8.324~8.345(d, 1H), 8.562~8.572(d, 1H), 8.828~8.839(d, 1H), 8.921(d, 1H), 9.272(d, 1H), 13.275(s, 1H) , HLPC-MS m / z: 306.1[M+1] + .
Embodiment 3
[0159] Example 3: N-allyl-2-bis(pyridin-2 base)methyleneamino-selenourea
[0160] Method is with embodiment 1, intermediate 4-allyl-3-selenocarbazide 1 H-NMR (400MHz, DMSO) δppm: 4.139 (m, 2H), 4.529 (m, 2H), 5.074~5.142 (m, 2H), 5.829~5.872 (m, 1H), 8.208 (m, 1H), 9.150 (m, 1H), product N-allyl-2-bis(pyridin-2yl)methyleneamino-selenourea, yellow solid 1 H-NMR (400MHz, DMSO) δppm: 4.3296~4.3584 (m, 2H), 5.1507~5.2222 (m, 2H), 5.8968~5.9396 (m, 1H), 7.4949~7.5299 (m, 2H), 7.6112 (m, 1H), 7.9706~8.0056 (m, 2H), 8.2648~8.2844 (d, 1H), 8.5801~8.5920 (d, 1H,) 8.8295~8.8421 (d, 1H), 9.4460~9.4754 (m, 1H), 13.5766 ( s, 1H). HLPC-MSm / z: 346.2[M+1] + .
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