A carbapenem derivative
A drug and compound technology, applied in the field of medicine, can solve problems such as poor absorption
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Embodiment 1
[0079] Example 1, (+)-(4R,5S,6S)-3-[[(3S,5S)-5-[[(aminosulfonyl)amino]methyl]-3-pyrrolidine]sulfur]-6 Preparation of -[(1R)-1-hydroxyethyl]-4-methyl-7-oxo-1-azabicyclo[3,2,0]hept-2-ene-2-carboxylic acid (Compound A)
[0080] Refer to the methods described in EP0632039, J.Antibiot.2006, 59(4):241-247 for preparation, and the full text is incorporated by reference. 36.1 g of doripenem monohydrate (compound A) was obtained, with a yield of 40.3%.
Embodiment 2
[0081] Example 2, (4R,5S,6S)-3-[[(3S,5S)-5-[[(aminosulfonyl)amino]methyl]-3-pyrrolidine]sulfur]-6-[(1R )-1-hydroxyethyl]-4-methyl-7-oxo-1-azabicyclo[3,2,0]hept-2-ene-2-carboxylic acid-(2-methoxy)ethyl Synthesis of Esters (Compound 1)
[0082] Doripenem monohydrate 4.39g (10mmol), 2-chloroethyl methyl ether 0.91ml (20mmol) and benzyltriethylammonium chloride 2.27g (20mmol) plus DMF 9ml, add diisopropyl Ethylamine 4.4ml (20mmol), react at 45°C for 4 hours, TLC detects that the reaction is complete, cool to 5°C, add 20ml of ethyl acetate, 20ml of water, adjust the pH to 4 with 1M citric acid solution under stirring, separate liquid, water The phase was adjusted to pH 7.6 with saturated potassium bicarbonate solution, extracted with ethyl acetate, washed with water, dried over anhydrous magnesium sulfate, evaporated to dryness, and the residue was prepared for column separation (ethanol-dichloromethane-acetone, 1:20:40), Evaporation to dryness gave 1.26 g (26.3%) of a yellowish ...
Embodiment 3
[0084] Example 3, (4R,5S,6S)-3-[[(3S,5S)-5-[[(aminosulfonyl)amino]methyl]-3-pyrrolidine]sulfur]-6-[(1R )-1-hydroxyethyl]-4-methyl-7-oxo-1-azabicyclo[3,2,0]hept-2-ene-2-carboxylic acid-(5-methyl-1,3 Synthesis of -dioxol-2-one) methyl ester (compound 2)
[0085] Doripenem monohydrate 4.39g (10mmol), 4-chloromethyl-5-ethyl-1,3-dioxol-2-one 2.97g (20mmol) and benzyltriethyl chloride Add 2.27g (20mmol) of ammonium and 9ml of DMF, add 4.4ml (20mmol) of diisopropylethylamine under stirring, react at 45°C for 4 hours, TLC detects that the reaction is complete, cool to 5°C, add 20ml of ethyl acetate and 20ml of water , adjusted to pH 4 with 1M citric acid solution under stirring, separated, the aqueous phase was adjusted to pH 7.6 with saturated potassium bicarbonate solution, washed with water after extraction with ethyl acetate, dried with anhydrous magnesium sulfate, evaporated to dryness, and the residue prepared column Separation (ethanol-dichloromethane-acetone, 1:20:40) was evap...
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