Dastorin primary alkylate derivative and its pharmaceutical composition, its preparation method and application
A technology of diastrin and alkyd ester, which is applied in the field of diasterin primary alkylate derivatives as a class of potent pancreatic lipase inhibitors, and can solve the problem of unseen diasterin primary alcohol Reports on the activity of ester derivatives and other issues
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Embodiment 1
[0037] 1 H-and 13 C-NMR is measured by Bruker AVANCE III-600, DRX-500 or AM-400, internal standard is TMS, wherein 1 H NMR measured at 400MHz, 500MHz and 600MHz, 13 C NMR was measured at 100MHz, 125MHz and 150MHz; mass spectrometry HREI-MS and EI-MS were determined by Finnigan-MAT90 mass spectrometer; HRESI-MS and ESI-MS were determined by API QSTAR Pulsari mass spectrometer; rotary evaporator: Buchi R-200 , R-201; DLSB5110 type low temperature reaction coolant circulation pump, IKARCT basic (safety control type) heating magnetic stirrer.
[0038] Column chromatography material: silica gel (80-100 mesh and 200-300 mesh) and prefabricated GF for column chromatography 254All TLC plates were produced by Qingdao Ocean Chemical Factory; Sephadex LH-20 was produced by Amersham Biosciences, Sweden; Chromatorex C-18 (40-75 μm) was produced by Fuji Silysia Chemicals, Japan. HPLC: Agilent1100, Zorbax SB-C18column, 5μm, 4.6mm×150mm; Prep-HPLC: Agilent1200, Zorbox SB-C18column, 5μm, 9...
Embodiment 2
[0098] In vitro experiments on the inhibition of pancreatic lipase by the compounds of the present invention:
[0099] 1. Determination of Drugs and Compounds
[0100] Determination compound is the first grade alkylate derivative of vibralactone gained in Example 1, totally 43 compounds; Positive drug is Orlistat (Orlistat, N-Formyl-L-leucine (1S)-1- [[(2S,3S)-3-hexyl-4oxo-2-oxetanyl]methyl]dodecyl ester) was purchased from Sigma; the compound and Orlistat were dissolved in dimethylsulfoxide (DMSO) and stored at 4°C.
[0101] 2. Reagents and solutions
[0102] (1) Reagents
[0103] Porcine pancreatic lipase (PPL) was purchased from Aladdin Reagent Company; p-nitrophenyl butyrate (p-NPB) and Tris were purchased from Sigma Company; D-PBS was purchased from Hyclone Company; anhydrous calcium chloride was purchased from Chengdu Kelong Chemical Reagent factory products.
[0104] (2) Solution
[0105] Tris buffer containing 100mM Tris, 5mM CaCl 2 , pH value is 7.0, and stored ...
Embodiment 3
[0122] The compound was prepared according to Example 1, and excipients were added according to the weight ratio of compound crystals and excipients at a ratio of 1:1, and then granulated and compressed into tablets.
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