1,4-phthalaldehyde

Onjezani 6.0 g wa sodium sulfide, 2.7 g wa sulfure ufa, 5 g wa sodium hydroxide ndi 60 ml ya madzi mu 250 ml atatu khosi botolo ndi reflux condenser ndi oyambitsa chipangizo, ndi kukweza kutentha kwa 80 ℃ poyambitsa.Mafuta a Yellow sulfure amasungunuka, ndipo yankho limakhala lofiira.Pambuyo pa refluxing kwa 1 h, yankho lakuda la sodium polysulfide limapezeka.

Onjezani 13.7 g wa p-nitrotoluene, 80 ml ya ethanol ya mafakitale, 0,279 g wa N, N-dimethylformamide ndi 2.0 g wa urea mu 250 ml botolo la khosi lachitatu loponyera, reflux condenser ndi chipangizo choyambitsa, kutentha ndi kusonkhezera. kusungunula p-nitrotoluene kupeza njira yopepuka yachikasu.Kutentha kumakwezedwa pang'onopang'ono mpaka 80 ℃ ndikusungidwa kosalekeza, yankho la sodium polysulfide lomwe lakonzedwa pamwambapa limatsitsidwa, ndipo yankho limasanduka buluu mwachangu, kenako limasanduka wobiriwira woderapo, ndipo pamapeto pake limasanduka bulauni.Imatsitsidwa mkati mwa maola 1.5-2.0, ndikusungidwa pa 80 ℃ chifukwa cha refluxing reaction kwa maola awiri.Mpweya distillation ikuchitika mofulumira.Pa nthawi yomweyi ya distillation, madzi a 100 ml amawonjezeredwa, 150 ml ya distillate amasonkhanitsidwa, ndipo pH mtengo ndi 7. Madzi otsalira amasungunuka ndi ayezi mwamsanga kuti awononge makristasi achikasu, omwe amachotsedwa ndi ether (30 ml × 5). ), amasungunuka ndi kuuma kuti apeze p-aminobenzaldehyde yellow solid.

Onjezani 5.89 paraformaldehyde, 13.2 g hydroxylamine hydrochloride ndi 85 ml madzi mu botolo la 250 ml la makosi atatu, kutentha ndi kusonkhezera kuti zonsezi zisungunuke kuti zisungunuke kuti zikhale zopanda mtundu, kenaka yikani 25.5 g sodium acetate hydrate, kusunga kutentha pa 80 ℃ ndi reflux kwa 15 min kuti mupeze formaldehyde oxime (10%) yankho lopanda mtundu.

Mu beaker 50 ml, onjezerani 3.5 g p-aminobenzaldehyde, 10 ml madzi, dontho 5 ml concentrated hydrochloric acid, ndipo pitirizani kusonkhezera.Zinthu zachikasu zowala zimasanduka zakuda mwachangu ndikusungunuka mosalekeza.Ikhoza kutenthedwa bwino (pansi pa 6 ℃) kuti isungunuke zonse.Uziziritsani mu madzi osambira amchere, ndipo kutentha kumatsika mpaka 5 ℃.Panthawi imeneyi, p-aminobenzaldehyde hydrochloride precipitates monga zabwino particles, ndi yankho amakhala phala.Pogwedezeka, 5-10 ℃ 5 ml ya sodium nitrite solution idadonthetsedwa mkati mwa mphindi 20, ndipo kusonkhezerako kunapitilizidwa kwa mphindi 20.40% sodium acetate solution idagwiritsidwa ntchito kusintha pepala lofiira la Congo kuti lisakhale ndale kuti lipeze yankho la mchere wa diazonium.

Sungunulani 0,7 g wa crystalline copper sulfate, 0,2 g wa sodium sulfite ndi 1.6 g wa sodium acetate hydrate mu 10% formaldehyde oxime solution, ndipo yankho limakhala lobiriwira.Pambuyo kudontha, sungani kutentha pang'ono kwa mphindi 30 kuti mutenge yankho la imvi, onjezerani 30 ml ya hydrochloric acid, kwezani kutentha mpaka 100 ℃, refluxe kwa ola limodzi, yankho likuwoneka lalalanje, distillation ya nthunzi, pezani cholimba choyera pang'ono, sefa ndi kuumitsa kuti mupeze mankhwala a p-benzaldehyde.Mankhwalawa adasinthidwanso ndi zosungunulira zosakanikirana za 1: 1 mowa ndi madzi.