Method for preparing bivalirudin through solid-liquid combination
A technology for bivalirudin and solution is applied in the field of preparing bivalirudin by solid-liquid combination, and achieves the effects of reducing the difficulty of purification, simple process operation, and being beneficial to industrial large-scale production.
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Embodiment 1
[0054] Example 1: Preparation of Boc-Pro-Gly-Gly-OH
[0055] Accurately weigh 79.8g (0.6mol) of Gly-Gly-OH and 127.2g (1.2mol) of sodium carbonate and dissolve in 1200mL of water, slowly add Boc-Pro-OSu THF solution at low temperature (2-8°C) ( 123.6g, 0.6mol) / 1000ml, stirred and reacted, TLC monitored the end point of the reaction, after the reaction was complete, the THF was evaporated off, and 10% citric acid aqueous solution was added under the ice-water bath to adjust the pH value of the solution to 2-3, 1000ml ethyl acetate extracted 3 Once, the organic phases were combined, concentrated by rotary evaporation to 1000ml, washed 3 times with 200ml saturated brine, dried over anhydrous sodium sulfate, crystallized by adding 2000ml of petroleum ether to obtain 148.4g of Boc-Pro-Gly-Gly-OH, with a yield of 75.2%.
Embodiment 2
[0056] Example 2: Preparation of Boc-Pro-Gly-Gly-OH
[0057] Accurately weigh 79.8g (0.6mol) of diglycine peptide Gly-Gly-OH and 63.6g (0.6mol) of sodium carbonate and dissolve it in 1200mL water, slowly add Boc-Pro-OSu THF solution at low temperature (2-8°C) ( 123.6g, 0.6mol) / 1000ml, stirred and reacted, TLC monitored the end point of the reaction, after the reaction was complete, the THF was evaporated off, and 10% citric acid aqueous solution was added under the ice-water bath to adjust the pH value of the solution to 2-3, 1000ml ethyl acetate extracted 3 Once, the organic phases were combined, concentrated by rotary evaporation to 1000ml, washed 3 times with 200ml saturated brine, dried over anhydrous sodium sulfate, crystallized by adding 2000ml of petroleum ether to obtain 145.2g of Boc-Pro-Gly-Gly-OH, with a yield of 73.5%.
Embodiment 3
[0058] Example 3: Preparation of Boc-Pro-Gly-Gly-Gly-Gly-OH
[0059] Accurately weigh 53.2g (0.4mol) of Gly-Gly-OH and 84.8g (0.8mol) of sodium carbonate and dissolve in 800mL of water, slowly add Boc-Pro-Gly-Gly-OSu at low temperature (2-8°C) THF solution (170.4g, 0.4mol) / 1000ml, stirred and reacted, TLC monitored the reaction end point, after the reaction was complete, the THF was evaporated off, and 10% citric acid aqueous solution was added under the ice-water bath to adjust the pH value of the solution to 2~3, 1000ml acetic acid Extract with ethyl ester 3 times, combine the organic phases, concentrate to 800ml by rotary evaporation, wash 3 times with 120ml saturated brine, dry over anhydrous sodium sulfate, add petroleum ether 1200ml for crystallization, and get Boc-Pro-Gly-Gly-Gly-Gly-Gly-OH 128.6g, yield 72.6%.
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