1,4-Phthalaldehyde

Yongeza i-6.0 g ye-sodium sulfide, i-2.7 g yomgubo wesulfure, i-5 g ye-sodium hydroxide kunye ne-60 ml yamanzi kwi-250 ml ye-flask ezintathu zentamo ene-reflux condenser kunye nesixhobo esishukumisayo, kwaye unyuse ubushushu bufike kuma-80 ℃ phantsi kokuxutywa.Umgubo wesulfure oMthubi uyanyibilika, kwaye isisombululo sijika sibe bomvu.Emva kwe-refluxing ye-1 h, isisombululo se-sodium polysulfide esimnyama esimnyama sifumaneka.

Yongeza i-13.7 g ye-p-nitrotoluene, i-80 ml ye-ethanol ye-industrial, i-0.279 g ye-N, i-N-dimethylformamide kunye ne-2.0 g ye-urea kwi-250 ml ye-flask enentamo ezintathu kunye ne-funnel yokulahla, i-condenser ye-reflux kunye nesixhobo esishukumisayo, ukushisa kunye nokugubha. ukunyibilikisa i-p-nitrotoluene ukufumana isisombululo esimthubi esikhanyayo.Xa iqondo lobushushu linyuswa kancinci ukuya kuma-80 ℃ kwaye ligcinwe lingaguquguquki, isisombululo se-sodium polysulfide esilungiselelwe kwinyathelo elingasentla siyehla, kwaye isisombululo sijike ngokukhawuleza sibe luhlaza okwesibhakabhaka, emva koko sijike luhlaza obumnyama sibe mdaka omnyama, kwaye ekugqibeleni sijike bubomvu bumdaka.Ithotywa phakathi kweeyure ze-1.5-2.0, ize igcinwe kwi-80 ℃ ukwenzela ukusabela kwe-refluxing iiyure ezi-2.I-steam distillation yenziwa ngokukhawuleza.Ngexesha elifanayo le-distillation, i-100 ml yamanzi yongezwa, i-150 ml ye-distillate iqokelelwa, kwaye ixabiso le-pH li-7. Ulwelo olushiyekileyo lupholiswe ngomkhenkce ngokukhawuleza ukukhupha iikristale ezikhanyayo eziphuzi, ezikhutshwe nge-ether (30 ml × 5). ), ingumphunga kwaye yomiswa ukufumana i-p-aminobenzaldehyde etyheli eqinileyo.

Yongeza i-5.89 paraformaldehyde, 13.2 g hydroxylamine hydrochloride kunye ne-85 ml yamanzi kwi-250 ml yeflask enentamo ezintathu, ubushushu kunye nokuvuselela ukuze ubenze bonke banyibilike ukufumana isisombululo esingenambala, wongeza i-25.5 g ye-sodium acetate hydrate, ugcine ubushushu kwi-80 ℃ kunye ne-reflux Imizuzu eyi-15 ukufumana i-formaldehyde oxime (10%) isisombululo esingenambala.

Kwi-beaker ye-50 ml, yongeza i-3.5 g p-aminobenzaldehyde, i-10 ml yamanzi, yehlisa i-5 ml egxininisiweyo ye-hydrochloric acid, kwaye uhlale uvuselela.Into etyheli ekhanyayo iba mnyama ngokukhawuleza kwaye inyibilika ngokuqhubekayo.Inokufudunyezwa ngokufanelekileyo (ngaphantsi kwe-6 ℃) ukuyinyibilikisa yonke.Yipholise kwibhafu yetyuwa yomkhenkce, kwaye iqondo lobushushu lehla liye ngaphantsi kwe-5 ℃.Ngeli xesha, i-p-aminobenzaldehyde hydrochloride iyancipha njengamasuntswana amahle, kwaye isisombululo siba yintlama.Ngaphantsi kokuvuselela, i-5-10 ℃ i-5 ml yesisombululo se-sodium nitrite yachithwa ngaphakathi kwe-20 min, kwaye ukuqhubela phambili kwaqhubeka malunga ne-20 min.I-40% isisombululo se-sodium acetate sasetyenziselwa ukulungelelanisa iphepha lokuhlola elibomvu laseCongo ukuba lingathathi hlangothi ukufumana isisombululo setyuwa ye-diazonium.

Dissolve 0.7 g ye-crystalline sulfate yethusi, i-0.2 g ye-sodium sulfite kunye ne-1.6 g ye-sodium acetate hydrate kwi-10% ye-formaldehyde isisombululo se-oxime, kwaye isisombululo sijika sibe luhlaza.Emva kokuvuza, gcina ubushushu obuphantsi kangangemizuzu engama-30 ukuze ufumane isisombululo esingwevu, yongeza i-30 ml egxininisiweyo ye-hydrochloric acid, phakamisa ubushushu ukuya kwi-100 ℃, i-refluxe ngeyure enye, isisombululo sibonakala si-orenji, i-distillation yomphunga, fumana okuqinileyo okumhlophe okutyheli kancinci, hluza kwaye womise ukufumana imveliso ekrwada ye-p-benzaldehyde.Imveliso yahlaziywa nge-solvent edibeneyo ye-1: 1 utywala kunye namanzi.