3339-73-9 3-Acide ya Phthalimidopropionic

1.1;2.1. mugihe cyo kubyitwaramo, reaction yakozwe kugeza igihe nta mazi yatonyanga, ubushyuhe bwamanutse bugera kuri 20 ° C, ubushyuhe bwagumishijwe kumasaha 2, kuyungurura, kuyungurura cake guteka Kuma 240.2 g ya phthalic anhydride alanine, HPLC yera 99.1%, umusaruro 97.7%.
I-16. azote, yashyizwemo igisubizo cya aside-aminopropanoic 3 (20 g, 224.48 mmol, 1.00 equiv) na 1,3- dihydro-2-benzofuran-l, 3-dione (33.28 g, 224,69 mmol, 1.00 equiv) muri acide acike (1,200 mL).Ibyo byakurikiwe no kongeramo acetate ya potasiyumu (66.0 g, mm 672.49 mmol, 3.00 equiv) mubice byinshi kuri 0 ° C.Igisubizo cyavuyemo cyashizwe kuri 3 h kuri 80 ° C mubwogero bwamavuta.Uruvange rwavuyemo rwibanze cyane mu cyuho.Igisubizo noneho cyazimye hiyongereyeho mL 150 y'amazi.Ibikusanyirizo byakusanyirijwe hamwe.Ibi byavuyemo 40 g (81%) ya 3- (l, 3-dioxo-2,3- dihydro-lH-isoindol-2-yl) acide protanoic nkikintu gikomeye cyera.R /.0.15 (muri Ethyl acetate: peteroli ether = 1: 1)
Uruvange rwa β-alanine (5.0 g, 0,06 mol), anhydride ya phthalic (8,7 g, 0,05 mol), na DMF (20 mL) yagaruwe nyuma yo gukurura 3 h.Uruvange rwavuyemo rwakonjeshejwe ubushyuhe bwicyumba, rusukwa mumazi-ice (~ 100 mL), hanyuma arungururwa no guswera.Agatsima kayunguruzo kwogejwe hamwe namazi (15 mL × 3), inzoga (3 mL × 3), na ether (10 mL × 2), hanyuma byumishwa muri vacuo kugirango utange 2e (9,9 g, 80%) nkumweru. bikomeye.
137.6 Intambwe ya 6: Uruvange rwa isobenzofuran-l, 3-dione (20 g, mmol 135) na aside aminopropanoque 3 (12 g, 135 mmol) yavanze kuri 170 ° C kuri 6h.Reba Ishusho 2. Iyo reaction irangiye, imvange yavanze n'amazi hanyuma ikuramo DCM (100 mL x 3).Ibice kama byahujwe byumye hejuru ya sodium sulfate ya anhydrous, irayungurura, hanyuma yibanda kumuvuduko muke kugirango itange 3- (l, 3-dioxoisoindolin-2-yl) aside protanoic 137g (20 g, 69%) nkikomeye cyera.
3-Acide ya Phthalimidopropanoic (4) Uruvange rwa anhydride ya phthalic (0,32 g, 2,2 mmol) na b-alanine (0,19 g, 2,2 mmol) yashyutswe mumashanyarazi afunguye kugeza 150˚C kuri 2 h.Nyuma yo gukonja kuri rt, H2O (5 mL) yongewemo hanyuma ivangwa rya reaction ryakuwe muri CH2Cl2 (2 X 20 mL).Igice kama cyumishijwe hejuru ya Na2SO4, kiyungurura no kwibanda kugirango gitange umweru wera (0,3 g) mumusaruro wa 62%;IR (KBr) 1711, 2954 cm-1;mp 140-141˚C.Igicuruzwa cyakoreshejwe mu ntambwe ikurikira nta yandi yeze.