Magaca:(S)-4-N-Boc-2-methylpiperazine
CAS:147081-29-6
Codsiga: Waa mid ka mid ah dhexdhexaadinta organic, sida AMG-510
Waxaa lagu heli karaa falcelin hal tallaabo oo S-2-Methylpiperazin ah
Dqayb ka mid ah diyaarinta:
Ku dar biyo (500g, 5w/w%) dhalada falcelinta.Ku dar (s) -2-methylpiperazine (100g, 998.4mmol, 1 u dhiganta) gudaha weelka falcelinta oo walaaqaya.Ku dar HCl (36% xal aqueous ah, 102.1g, 1008mmol, 1.01 u dhiganta) iyo methanol (200g) ku shub weelka falcelinta oo walaaqaya.Ku dar xalalka boc2o (222g, 1008mmol, 1.01 u dhiganta) ee methanol (200g) hoos u dhig ku shub weelka falcelinta 15-25 ℃, ka dibna walaaq 20-30 ℃ 18 saacadood.Ku uumi waxa ku jira weelka si ay u engegaan meel faaruq ah 40-50 ℃ si aad u samaysato hadhaa.Biyaha (500g) ayaa lagu daray hadhaagii, isku dar ah ayaa la walaaqay 1 saac.Isku darka waa la sifeeyay oo adkaha la ururiyay waxaa lagu dhaqaay biyo (50g).Ka soo saar sifaynta aqueous leh ethyl acetate (500ml).Ku hagaaji wejiga aqueous ee la soo saaray 30% naoh ilaa pH ka badan 12, ka dibna ku soo saar saddex jeer ethyl acetate (500ml).Marxaladda dabiiciga ah waxaa lagu dhaqay laba jeer brine (500g) ka dibna lagu qallajiyey Na2SO4.Isku darka la qalajiyey ayaa la sifeeyay oo adkaha la ururiyey waxaa lagu dhaqay ethyl acetate (100ml).Shaandhaynta waxa lagu ururiyey qallayl meel faaruq ah oo ah 50-60 ℃ waxaana lagu sii daray faakuum sare (5mm Hg) at 65-75 ℃ 3 saacadood si loo helo (s) -4-n-tert butoxycarbonyl-2-methylpiperazine.Nadiifintu waxay ahayd 97.7%, nuxurku wuxuu ahaa 95.9%, waxsoosaarkuna wuxuu ahaa 76.4%.
Waqtiga boostada: Juun-27-2022