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Dzina:(S) -4-N-Boc-2-methylpiperazine

CAS:147081-29-6

Ntchito: Ndi imodzi mwazinthu zapakatikati, monga AMG-510

Itha kuchitidwa ndi sitepe imodzi ya S-2-Methylpiperazion

DKukonzekera:

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Onjezani madzi (500g, 5w/w%) mu botolo lochita.Onjezani (s) -2-methylpiperazine (100g, 998.4mmol, 1 yofanana) mu botolo lomwe likuyambitsa ndi kusonkhezera.Onjezani HCl (36% yankho lamadzimadzi, 102.1g, 1008mmol, 1.01 ofanana) ndi methanol (200g) mu botolo lamadzimadzi ndikugwedeza.Onjezani njira ya boc2o (222g, 1008mmol, 1.01 yofanana) mu methanol (200g) dontho ndi dontho mu botolo lomwe limakhala pa 15-25 ℃, kenako ndikuyambitsa 20-30 ℃ kwa maola 18.Sungani zomwe zili mu botolo kuti ziume pansi pa vacuum pa 40-50 ℃ kuti mupange zotsalira.Madzi (500g) adawonjezeredwa ku zotsalirazo ndipo kusakaniza kunalimbikitsidwa kwa ola limodzi.Kusakaniza kumasefedwa ndipo zolimba zomwe zidasonkhanitsidwa zimatsukidwa ndi madzi (50g).Chotsani kusefa kwamadzi ndi ethyl acetate (500ml).Sinthani gawo lamadzi lotulutsidwa ndi 30%naoh kukhala pH yopitilira 12, kenako ndikuchotsani katatu ndi ethyl acetate (500ml).The organic gawo anasambitsidwa kawiri ndi brine (500g) ndiyeno zouma ndi anhydrous Na2SO4.Zosakaniza zouma zidasefedwa ndipo zolimba zomwe zidasonkhanitsidwa zidatsukidwa ndi ethyl acetate (100ml).Sefayi idakhazikika pakuuma mu vacuum pa 50-60 ℃ ndikukhazikikanso mu vacuum yayikulu (5mm Hg) pa 65-75 ℃ kwa maola atatu kuti ipeze (s) -4-n-tert butoxycarbonyl-2-methylpiperazine.Kuyera kunali 97.7%, zomwe zinali 95.9%, ndipo zokolola zinali 76.4%.


Nthawi yotumiza: Jun-27-2022