1,5-diazabicyclo[5,3,0]decane ketone amino acid derivative as well as preparation method and application thereof
A kind of technology of diazabicyclo and derivatives, applied in 1 field
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Embodiment 1
[0038] Preparation of Compound I-1
[0039] Reaction route:
[0040]
[0041] Specific preparation process:
[0042] 1. Preparation of (2S,5R)-5-(((tert-butyldimethylchloride) oxo)methyl) tetrahydropyrrole-2-carboxylate
[0043]
[0044] At room temperature, the raw material (2S,5R)-5-(hydroxymethyl)tetrahydropyrrole-2-carboxylate methyl ester (1.50g, 8.67mmol) was dissolved in 10mL of dichloromethane, and tert-butyl was added under stirring Dimethylchlorosilane (1.56g, 10.40mmol) and triethylamine (2.62g, 26.01mmol) were reacted at room temperature for 6h until the reaction was complete as monitored by TLC. It was extracted three times with DCM and water, and the combined organic phases were washed with saturated sodium chloride solution. It was dried over anhydrous sodium sulfate, filtered, concentrated, separated and concentrated by column chromatography to obtain 1.77 g of a colorless oil, with a yield of 71%. TLC (ethyl acetate:petroleum ether=2:1) Rf=0.2.
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Embodiment 2
[0071] Preparation of Compound I-2
[0072]
[0073] (700mg, 1.8mmol) of 2-((tert-butoxycarbonyl)amino)-3-((2-nitrophenyl)sulfonamido)propionic acid and 5-(((tert-butyl Dimethylchloro)oxo)methyl)tetrahydropyrrole-2-carboxylate ethyl ester (500mg, 1.74mmol), using Method 2 to obtain light yellow oily condensation product 2-((tert-butoxycarbonyl)amino) -3-((2-nitrophenyl)sulfonamido)propionyl)-5-(((tert-butyldimethylsilyl)oxo)methyl)tetrahydropyrrole-2-carboxylic acid ethyl ester (1.01 g, 1.53 mmol).
[0074] 2-((tert-butoxycarbonyl)amino)-3-((2-nitrophenyl)sulfonamido)propionyl)-5-(((tert-butyldimethylsilyl)oxo)methyl ) Ethyl tetrahydropyrrole-2-carboxylate Using method three to obtain light yellow oil 2-((tert-butoxycarbonyl)amino)-3-((2-nitrophenyl)sulfonamido)propionyl)- Ethyl 5-(hydroxymethyl)tetrahydropyrrole-2-carboxylate. (735 mg, 1.35 mmol).
[0075] 2-((tert-butoxycarbonyl)amino)-3-((2-nitrophenyl)sulfonamido)propionyl)-5-(hydroxymethyl)tetrahydropyrrole-2-carb...
Embodiment 3
[0078] Preparation of Compound I-6
[0079]
[0080] 2-Oxo-3-((tert-butoxycarbonyl)amino)-1,5-diazabicyclo[5,3,0]decane-10-carboxylic acid ethyl ester (100mg, 0.29mmol) was placed in React in methanolic hydrochloric acid solution for 2 hours at room temperature, spin dry the reaction solution, extract three times with ethyl acetate and saturated sodium bicarbonate solution, collect the organic phase, dry over sodium sulfate, and spin dry to obtain a colorless oily 2-oxo-3-amino- Ethyl 1,5-diazabicyclo[5,3,0]decane-10-carboxylate (78 mg, 0.28 mmol).
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