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(6R,7R)-3-[2-(2-Amino-ethylsulfanylmethyl)-pyridin-3-ylsulfanyl]-7-{2-(5-amino-[1,2,4]thiadiazol-3-yl)-2-[(Z)-hydroxyimino]-acetylamino}-8-oxo-5-thia-1-aza-bicyclo[4.2.0]oct-2-ene-2-carboxylic acid[ No CAS ]
(6R,7R)-1-aza-3-<((2)H3)-methyl>-7-amino-<(5R)-5-N-p-methoxybenzyloxycarbonylamino-5-p-methoxybenzyloxycarbonylpentanamido>-8-oxo-5-thiabicyclo<4.2.0>oct-2-ene-2-carboxylic acid benzhydryl ester[ No CAS ]
To the reactor was added 100 ml of a dichloromethane solvent,Temperature control is 25C ,Accurately weigh 20.00g <strong>[53994-69-7]7-ACCA</strong> and added to the reactor, A <strong>[53994-69-7]7-ACCA</strong> solution was obtained, Temperature control is 30C , Add compoundSilylating agents, The complex silanization reagent comprises 10.00 g of trimethylchlorosilane, 9.40 g of hexamethyldisilazane, 0.200 g of N,O-bis-trimethylsilylacetamide, and the reaction temperature was controlled to 46 C. The reaction was started under reflux and the reaction was cooled to -15 C.
Formulated NaBH4 aqueous solution: 16.56g H2O + 4.73g NaBH4 (0.125mol),Stir and dissolve, and control the temperature between 5 and 10 C.Into a 500 mL four-necked flask, put methanol (117.35 g), water (117.35 g), and <strong>[53994-69-7]7-ACCA</strong> (23.47 g, 0.10 mol).Stir and control the temperature from 15 to 25 C. Add 5% ammonia water dropwise to adjust the pH to 7.0 to 7.5. After the pH is stable, stir for about 0.5h until the reaction solution is clear.Add nickel chloride hexahydrate (2.38 g, 0.01 mol) to the reaction solution, and dropwise add the prepared NaBH4 aqueous solution.It took about 2 to 3 hours. After dripping and stirring for 12 hours, the residue of <strong>[53994-69-7]7-ACCA</strong> detected by HPLC was less than 1%, and the reaction was completed.Add acetone (117.35g) to the solution after the reaction, and adjust the pH to 4.0-4.5 with 10% hydrochloric acid at 15-25 C.The obtained filter cake was dried under vacuum at 50 C. for 6 h to obtain compound A (21.58 g),Its molar yield was 91.18% and its HPLC purity was 99.35%.
With sodium hydrogencarbonate In water; acetone at 4 - 19℃; for 4h;
4 Example 4 Operation example of TM1kTM1y synthesis
General procedure: Add 7-AXCA (5mmol),5mL of acetone and 1mL of water,Stir at room temperature,Add sodium bicarbonate (1.26g, 1.5mmol),In an ice salt bath, add acid chloride (1.0 mmol) dropwise,Stir. TLC monitors the progress of the reaction.After the reaction is complete,Add ice-cold 2NHCl to adjust pH=7,Spin off the solvent acetone,Freeze to precipitate solids,Add ice-cold 2NHCl to adjust pH=3,A large amount of solid precipitated out.Suction filtration, drying,Obtain solid TM1kTM1y.The experimental results are shown in Table 7.
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