1,4-Phthalaldehyde

Faka u-6.0 g we-sodium sulfide, u-2.7 g wempushana yesibabule, u-5 g we-sodium hydroxide no-60 ml wamanzi eflaskini engu-250 ml enentamo emithathu ene-reflux condenser kanye nomshini onyakazayo, bese ukhuphula izinga lokushisa libe ku-80 ℃ ngaphansi kokunyakaziswa.Impushana yesulfure Ephuzi iyancibilika, bese isixazululo sibe bomvu.Ngemuva kwe-refluxing ihora elingu-1, isisombululo se-sodium polysulfide esimnyama esimnyama sitholakala.

Faka u-13.7 g we-p-nitrotoluene, u-80 ml we-ethanol yezimboni, u-0.279 g we-N, i-N-dimethylformamide no-2.0 g we-urea ku-250 ml weflask enezintamo ezintathu nefaneli yokudonsa, i-reflux condenser kanye nesisetshenziswa esinyakazayo, ukushisa nokunyakazisa. ukuncibilikisa i-p-nitrotoluene ukuze uthole isixazululo esiphuzi esikhanyayo.Lapho izinga lokushisa likhuphuka kancane kancane libe ngu-80 ℃ futhi ligcinwa lingashintshile, isixazululo se-sodium polysulfide esilungiselelwe esinyathelweni esingenhla siyehliswa, bese isixazululo sishintsha ngokushesha sibe luhlaza okwesibhakabhaka, bese sishintsha sibe luhlaza okotshani sibe nsundu ngokumnyama, futhi ekugcineni sibe nsundu ngokubomvu.Yehliswa phakathi kwamahora angu-1.5-2.0, bese igcinwa ku-80 ℃ ukuze iphendule i-refluxing amahora angu-2.I-Steam distillation yenziwa ngokushesha.Ngesikhathi esifanayo se-distillation, amanzi angu-100 ml ayengeziwe, i-150 ml ye-distillate iyaqoqwa, futhi inani le-pH liyi-7. Uketshezi olusele lupholiswa ngeqhwa ngokushesha ukuze kuqhume amakristalu aphuzi aphuzi, akhishwa nge-ether (30 ml × 5). ), iyahwamuka futhi yomiswa ukuze kutholakale okuqinile okuphuzi kwe-p-aminobenzaldehyde.

Faka i-5.89 paraformaldehyde, 13.2 g hydroxylamine hydrochloride kanye namanzi angu-85 ml eflaskini engu-250 ml enezintamo ezintathu, fudumeza futhi ugovuze ukuze zonke zincibilike ukuze uthole isixazululo esingenambala, bese wengeza u-25.5 g we-sodium acetate hydrate, ugcine izinga lokushisa liku-80 ℃ bese uphinde uphendule 15 min ukuthola i-formaldehyde oxime (10%) isixazululo esingenambala.

Ebhikeni elingu-50 ml, engeza u-3.5 g we-p-aminobenzaldehyde, u-10 ml wamanzi, wehlisa u-5 ml we-hydrochloric acid egxilile, bese uqhubeka ugqugquzela.Into ephuzi ngokukhanyayo iba mnyama ngokushesha futhi incibilike ngokuqhubekayo.Ingashiswa kahle (ngaphansi kuka-6 ℃) ukuze incibilike yonke.Yipholise kubhavu we-ice salt, futhi izinga lokushisa liyehla libe ngaphansi kuka-5 ℃.Ngalesi sikhathi, i-p-aminobenzaldehyde hydrochloride idlula njengezinhlayiya ezinhle, futhi isixazululo siba sinama.Ngaphansi kokugqugquzelwa, i-5-10 ℃ 5 ml yesisombululo se-sodium nitrite yaconsa phakathi nemizuzu engama-20, futhi ukugqugquzela kwaqhubeka cishe imizuzu engama-20.Isixazululo esingu-40% se-sodium acetate sasetshenziswa ukulungisa iphepha lokuhlola elibomvu laseCongo ukuze lingathathi hlangothi ukuze kutholwe isixazululo sikasawoti we-diazonium.

Chaza u-0.7 g we-crystalline copper sulfate, u-0.2 g we-sodium sulfite kanye no-1.6 g we-sodium acetate hydrate ube yisisombululo se-formaldehyde oxime esingu-10%, bese isixazululo sibe luhlaza.Ngemuva kokuconsa, gcina izinga lokushisa eliphansi imizuzu engama-30 ukuze uthole isisombululo esimpunga, engeza u-30 ml we-hydrochloric acid egxilile, ukhuphule izinga lokushisa libe ngu-100 ℃, i-refluxe ihora eli-1, isixazululo sibonakala siwolintshi, i-steam distillation, thola okuqinile okumhlophe okuphuzi kancane, hlunga futhi wome ukuze uthole umkhiqizo ongahluziwe we-p-benzaldehyde.Umkhiqizo waphinde wahlanganiswa ne-solvent exubile ye-1: 1 utshwala namanzi.