inoa:(S)-4-N-Boc-2-methylpiperazine
CAS:147081-29-6
Noi: ʻO ia kekahi o nā mea waena, e like me AMG-510
Hiki ke loaʻa iā ia ma ka hopena hoʻokahi o ka S-2-Methylpiperazion
Detail o ka hoomakaukau ana:
E hoʻohui i ka wai (500g, 5w/w%) i loko o ka ʻōmole hopena.E hoʻohui i (s) -2-methylpiperazine (100g, 998.4mmol, 1 like) i loko o ka pahu pane me ka hoʻoulu ʻana.E hoʻohui i ka HCl (36% wai wai, 102.1g, 1008mmol, 1.01 like) a me ka methanol (200g) i loko o ka pahu pane me ka hoʻoulu ʻana.E hoʻohui i ka solution o ka boc2o (222g, 1008mmol, 1.01 equivalent) i loko o ka methanol (200g) kulu i kēlā me kēia kulu i loko o ka pahu hopena ma 15-25 ℃, a laila hoʻoulu i ka 20-30 ℃ no 18 mau hola.E hoʻoheheʻe i nā mea i loko o ka ipu a maloʻo ma lalo o ka momi ma 40-50 ℃ e hana i ke koena.Hoʻohui ʻia ka wai (500g) i ke koena a hoʻoulu ʻia ka hui ʻana no 1 hola.Ua kānana ʻia ka hui ʻana a holoi ʻia nā mea paʻa i hōʻiliʻili ʻia me ka wai (50g).Wehe i ka wai kānana me ka ethyl acetate (500ml).E hoʻoponopono i ka ʻāpana wai i unuhi ʻia me 30%naoh i kahi pH ʻoi aku ma mua o 12, a laila unuhi ʻekolu manawa me ka ethyl acetate (500ml).Ua holoi ʻia ka ʻāpana organik ʻelua me ka brine (500g) a laila maloʻo me ka Na2SO4 anhydrous.Ua kānana ʻia ka hui maloʻo a holoi ʻia ka paʻakai i hōʻiliʻili ʻia me ka ethyl acetate (100ml).Hoʻopili ʻia ka filtrate i ka maloʻo i loko o ka ʻūhā ma 50-60 ℃ a hoʻopaʻa ʻia i loko o ka ʻūhā kiʻekiʻe (5mm Hg) ma 65-75 ℃ no 3 mau hola e loaʻa ai (s) -4-n-tert butoxycarbonyl-2-methylpiperazine.ʻO ka maʻemaʻe he 97.7%, he 95.9% ka maʻi, a he 76.4% ka hua.
Ka manawa hoʻouna: Iune-27-2022