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A carbetocin and solution technology, applied in the field of solid-liquid phase combination synthesis of polypeptides, can solve the problems of high purification cost and low yield, and achieve the effects of reduced purification difficulty, good yield and optimized extraction ratio
Active Publication Date: 2016-06-01
GL BIOCHEM SHANGHAI
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[0010] In order to increase the synthesis yield of carbetocin and improve the quality of synthesis, the present invention discloses a convenient, quick and easy-to-large-scale
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Embodiment 1
[0028] Embodiment 1: the synthesis of Fmoc-Gly-amino resin, refer to figure 1 ,
[0029] Add 142 grams of amino resin, with a substitution degree of 0.4 mmol / g, into the solid-phase reaction column, add DCM to swell the resin for 30 minutes, add 34 grams of Fmoc-Gly-OH, 43 grams of HATU,
[0030] 17 g of HOAt was dissolved in DMF and cooled to 5 °C, reacted with nitrogen gas, added 13.7 g of TMP, reacted at room temperature for 50 minutes, washed with DMF for 3 times, and washed with DCM and methanol for 3 times.
[0031] The solid-phase reactor is a sandy funnel, the lower part of which is connected to a tee, one end of the tee is connected to a nitrogen bottle, and the other end of the tee is connected to a suction filter bottle and a vacuum pump, which is convenient for nitrogen and suction filtration.
Embodiment 2
[0032] Embodiment 2: the synthesis of Fmoc-Gly-amino resin, refer to figure 1 ,
[0033]Add 142 grams of amino resin, with a substitution degree of 1.2 mmol / g, into the solid-phase reaction column. After adding DCM to swell the resin for 30 minutes, add 102 grams of Fmoc-Gly-OH, 129 grams of HATU,
[0034] 51 g of HOAt was dissolved in its own DMF and cooled to 5°C, reacted with nitrogen gas, added 41.1 g of TMP, reacted at room temperature for 50 minutes, washed with DMF for 3 times, and washed with DCM and methanol for 3 times alternately.
Embodiment 3
[0035] Embodiment 3, with reference to figure 1 , amino resin substitution degree is 0.8mmol / g, coupling agent DIC / HOBt, all the other are the same as embodiment 1.
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Abstract
The invention relates to a method for synthesizing polypeptide by combining solid and liquid phases, in particular to a preparation method of Carbetocin, and mainly solves the technical problems that the existing preparation method is low in yield and high in purifying cost. The invention adopts a technical scheme as follows: the preparation method of the Carbetocin comprises the following steps: 1) sequentially coupling amino resin with Fmoc-Gly-OH, Fmoc-Leu-OH, Fmoc-Pro-OH, Fmoc-Cys(Alloc)-OH, Fmoc-Asn(Trt)-OH, Fmoc-Gln(Trt)-OH and Fmoc-Ile-OH by using a coupling agent to obtain resin polypeptide; 2) performing de-cysteine protection; 3) carrying out reaction with 4-halogeno butyric acid under an alkaline condition, and coupling with H-Tyr(OMe)-OtBu; 4) cutting polypeptide, and performing ring closure on a liquid phase; 5) performing efficient countercurrent chromatographic purification on crude peptide, and lyophilizing to obtain the Carbetocin. The preparation method is mainly used for preparing the Carbetocin.
Description
technical field [0001] The invention relates to a method for combining solid-liquid phases to synthesize polypeptides, in particular to a method for preparing carbetocin. Background technique [0002] To prevent uterine atony and postpartum hemorrhage, in addition to massaging the uterus, drugs that contract the uterus are mainly used. Oxytocin, ergonovine, and prostaglandin preparations are commonly used as uterotonic agents, and each drug has its advantages and disadvantages. Oxytocin is the most widely used, with the advantages of fast onset of action, safety, and less side effects, but the disadvantage of short action time, with a half-life of 1 to 6 minutes, and its function depends on the oxytocin receptor in the body. , Unrestricted increase the dosage but the effect is not good, and side effects appear, the total amount of 24h should be controlled within 60u. For these reasons, oxytocin sometimes has a limited effect. Ergonovine has a contractile effect on the ute...
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