中国兽药杂志
中國獸藥雜誌
중국수약잡지
CHINESE JOURNAL OF VETERINARY DRUG
2014年
10期
22-25
,共4页
薛克友%葛健%沈华%张卫元%刘洁
薛剋友%葛健%瀋華%張衛元%劉潔
설극우%갈건%침화%장위원%류길
盐酸沃尼妙林%合成%截短侧耳素
鹽痠沃尼妙林%閤成%截短側耳素
염산옥니묘림%합성%절단측이소
valnemulin hydrochloride%synthesis%pleuromutilin
以精制的截短侧耳素为原料,经对甲苯磺酰氯磺化后,与二甲基半胱胺盐酸盐反应,制得截短侧耳素半胱胺取代物;另外由D-缬氨酸、乙酰乙酸甲酯和氢氧化钾反应制得( R)-2-(1-甲氧羰基-2-烯丙基)氨基-3-甲基丁酸钾,经氯甲酸乙酯活化后与截短侧耳素半胱胺取代物反应,最后通过调节pH值,经反相萃取后,冻干得盐酸沃尼妙林,总收率为69%,所得产品按照EP6.0进行了质量检测,产品具有含量高、杂质少等优点。
以精製的截短側耳素為原料,經對甲苯磺酰氯磺化後,與二甲基半胱胺鹽痠鹽反應,製得截短側耳素半胱胺取代物;另外由D-纈氨痠、乙酰乙痠甲酯和氫氧化鉀反應製得( R)-2-(1-甲氧羰基-2-烯丙基)氨基-3-甲基丁痠鉀,經氯甲痠乙酯活化後與截短側耳素半胱胺取代物反應,最後通過調節pH值,經反相萃取後,凍榦得鹽痠沃尼妙林,總收率為69%,所得產品按照EP6.0進行瞭質量檢測,產品具有含量高、雜質少等優點。
이정제적절단측이소위원료,경대갑분광선록광화후,여이갑기반광알염산염반응,제득절단측이소반광알취대물;령외유D-힐안산、을선을산갑지화경양화갑반응제득( R)-2-(1-갑양탄기-2-희병기)안기-3-갑기정산갑,경록갑산을지활화후여절단측이소반광알취대물반응,최후통과조절pH치,경반상췌취후,동간득염산옥니묘림,총수솔위69%,소득산품안조EP6.0진행료질량검측,산품구유함량고、잡질소등우점。
The refined pleuromutilin reacted with p - toluene sulfonyl chloride and dimethyl cysteamine hydrochloride to prepare cysteamine substituent. Another D-valine and methyl acetoacetate reacted with potassium hydroxide to obtain ( R)-2-( 1-methoxycarbonyl-2-allyl) amino-3-methylbut-potassium. After it was activated by ethyl chloroformate, the product reacted with pleuromutilin cysteamine substitution, finally, adjusted the pH value and inverted extraction to obtain valnemulin hydrochloride with the total yield of 69%. The product was tested according to EP6.0 which had high content and low impurities.