3339-73-9 3-Phthalimidopropionic acid

1.1;2.1. inta lagu guda jiro falcelinta, falcelinta ayaa la fuliyay ilaa aan biyo hoos u dhicin, heerkulka ayaa hoos loo dhigay ilaa 20 ° C, heerkulka waxaa lagu hayaa 2 saacadood, sifaynta nuugista, dubista keega filter qallaji 240.2 g of phthalic anhydride alanine, HPLC daahirnimada 99.1%, wax-soo-saarka 97.7%.
I-16.1 Synthesis of 3- (l,3-dioxo-2,3-dihydro-lH-isoindol-2-yl)propanoic acid Gal 3-L 4-luug oo weel xaga hoose ah oo la safeeyey laguna ilaaliyo jawi aan firfircoonayn nitrogen, ayaa la dhigay xal 3-aminopropanoic acid (20 g, 224.48 mmol, 1.00 equiv) iyo 1,3-dihydro-2-benzofuran-l,3-dione (33.28 g, 224.69 mmol, 1.00 equiv) ee acetic acid (1,200 ml).Tan waxaa ku xigtay in lagu daro potassium acetate (66.0 g, 672.49 mmol, 3.00 equiv) dhowr qaybood oo ah 0 °C.Xalka ka dhashay waxaa lagu walaaqay 3 h 80 ° C ee qubeyska saliidda.Isku darka ka dhashay wuxuu ku ururay faakuum hoostiisa.Dareen-celinta ayaa markaa la demiyay iyadoo lagu daray 150 ml oo biyo ah.Cuntooyinka adag waxaa lagu soo ururiyay sifeyn.Tani waxay keentay 40 g (81%) ee 3- (l,3-dioxo-2,3-dihydro-lH-isoindol-2-yl)propanoic acid sida adag cad.R/0.15 (ee ethyl acetate: petroleum ether = 1: 1)
Isku darka β-alanine (5.0 g, 0.056 mol), phthalic anhydride (8.7 g, 0.059 mol), iyo DMF (20 mL) ayaa dib loo soo celiyay iyada oo la walaaqayo 3 saacadood.Isku darka ka dhashay ayaa la qaboojiyey heerkulka qolka, lagu shubay baraf-biyo (~ 100 mL), ka dibna lagu sifeeyay nuugista.Keega shaandhada ayaa si isdaba joog ah loogu dhaqay biyo (15 mL × 3), aalkolo (3 mL × 3), iyo ether (10 mL × 2), ka dibna la qalajiyey vacuo si loo siiyo 2e (9.9 g, 80%) sida cad. adag.
137.6 Tallaabada 6: Isku dar ah isobenzofuran-l,3-dione (20 g, 135 mmol) iyo 3-aminopropanoic acid (12 g, 135 mmol) ayaa lagu walaaqay 170 ° C ilaa 6h.Fiiri sawirka 2. Marka falcelinta la dhammeeyo, isku darka ayaa lagu qasi jiray biyo waxaana lagu soo saaray DCM (100 mL x 3).Lakabyada organic-ga ah ee la isku daray ayaa lagu qallajiyey sodium sulfate anhydrous, la sifeeyay, oo la saaray cadaadis la dhimay si loo siiyo 3- (l,3-dioxoisoindolin-2-yl) propanoic acid 137g (20 g, 69%) sida adag cad.
3-Phthalimidopropanoic acid (4) Isku dar ah phthalic anhydride (0.32 g, 2.2 mmol) iyo b-alanine (0.19 g, 2.2 mmol) ayaa lagu kululeeyay weel furan ilaa 150˚C muddo 2 saacadood ah.Kadib qaboojinta rt, H2O (5 mL) ayaa lagu daray oo isku darka falcelinta waxaa laga soo saaray CH2Cl2 (2 X 20 mL).Lakabka dabiiciga ah ayaa lagu qallajiyey Na2SO4, la sifeeyay oo la saaray si loo siiyo cad cad (0.3 g) ee 62% dhalidda;IR (KBr) 1711, 2954 cm-1;mp 140-141˚C.Alaabta ayaa loo isticmaalay tallaabada xigta iyada oo aan la nadiifin.