Compound for treatment of severe pancreatitis and preparation method thereof
A compound and selected technology, applied in the field of medicine, can solve the problems of poor solubility of emodin and affecting drug efficacy, etc.
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Embodiment 1
[0039] Example 1: 1-{2-(3,7-Dimethyl-5-oxo-5H-thiazolo[3,2-a]pyrimidin-6-yl)-2-oxoethyl)-3 -(pyridin-2-yl)urea (compound 1)
[0040]
[0041] Step 1) Add polyphosphoric acid (20.0 g, 183.0 mmol) into a three-necked flask equipped with a condenser, a thermometer and a nitrogen outlet. The flask was heated to about 70°C to obtain an easily stirred liquid. With stirring, 4-methyl-1,3-thiazol-2-amine (4.0 g, 35.0 mmol) was added in small portions. The temperature of the solution was slowly increased to 78°C while stirring. Then, ethyl acetoacetate (4.9 g, 42.0 mmol) was slowly dropped in through the dropping funnel, and the mixture was heated to 110° C. under nitrogen, and reacted for 6 hours. The reaction mixture was cooled, and water (40 mL) and ethyl acetate (100 mL) were added. The mixture was stirred until all solids were dissolved. Separate the organic layer, extract the aqueous layer with ethyl acetate, and combine the organic layers, and wash the organic layer with...
Embodiment 2
[0047] Example 2: 1-{2-(7-fluoromethyl-3-methyl-5-oxo-5H-oxazolo[3,2-a]pyrimidin-6-yl)-2-oxoethyl base)-3-(quinolin-2-yl)urea (compound 2)
[0048]
[0049] According to the method of Example 1, replace 4-methyl-1,3-thiazol-2-amine with 4-methyl-1,3-oxazol-2-amine, and use 4-fluoro-3-oxobutanoic acid Ethyl acetoacetate was replaced by ethyl acetoacetate, and 1-(pyridin-2-yl)urea was replaced by 1-(quinolin-2-yl)urea to give a light yellow solid with a total yield of 48%, ESI-MS: 410.12 [M +H] + .
Embodiment 3
[0050] Example 3: 1-{2-(7-cyclopropyl-3-methyl-5-oxo-5H-thiazolo[3,2-a]pyrimidin-6-yl)-2-oxoethyl )-3-(piperidin-4-yl)urea (compound 3)
[0051]
[0052] According to the method of Example 1, replace ethyl acetoacetate with ethyl 4-cyclopropyl-3-oxobutanoate, replace 1-(pyridin-2-yl) with 1-(piperidin-4-yl)urea Urea, a light yellow solid was obtained, the total yield was 55%, ESI-MS: 390.15[M+H] + .
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