1,4-Phthalaldehyde

Ongeramo 6.0 g ya sodium sulfide, 2,7 g yifu ya sulfure, g 5 ya hydroxide ya sodium na ml 60 yamazi muri ml 250 ya flask eshatu yizosi hamwe na kondenseri ya reflux hamwe nigikoresho gikurura, hanyuma uzamure ubushyuhe bugere kuri 80 ℃ munsi yo gukurura.Ifu ya sulfure yumuhondo irashonga, kandi igisubizo gihinduka umutuku.Nyuma yo kugaruka kuri 1 h, habonetse igisubizo cyumutuku sodium polysulfide.

Ongeramo 13,7 g ya p-nitrotoluene, ml 80 ya Ethanol yinganda, 0.279 g ya N, N-dimethylformamide na g g 2,2 ya urea muri ml 250 ya flask yamajosi 250 hamwe na feri ya feri, kondereseri igaruka hamwe nigikoresho gikurura, ubushyuhe no gukurura gushonga p-nitrotoluene kugirango ubone igisubizo cyumuhondo cyoroshye.Iyo ubushyuhe buzamutse buhoro buhoro bugera kuri 80 ℃ kandi bugakomeza guhoraho, igisubizo cya sodium polysulfide cyateguwe muntambwe yavuzwe haruguru kiragabanuka, kandi igisubizo gihinduka ubururu, hanyuma gihinduka icyatsi kibisi cyijimye cyijimye, amaherezo gihinduka umutuku wijimye.Iramanuka mumasaha 1.5-2.0, hanyuma ikabikwa kuri 80 ℃ kugirango igarure reaction kumasaha 2.Gukuramo amavuta bikorwa vuba.Mugihe kimwe cyo gusibanganya, hongewemo amazi 100, ml 150 ya distillate, hamwe na pH agaciro ka 7. Amazi asigaye akonjeshwa nurubura vuba kugirango agabanye kristu yumuhondo yoroheje, ikurwamo na ether (30 ml × 5 ), guhumeka no gukama kugirango ubone p-aminobenzaldehyde yumuhondo ukomeye.

Ongeramo 5.89 paraformaldehyde, 13.2 g hydroxylamine hydrochloride na 85 ml mumazi ya 250 250 flask yamajosi atatu, shyushya hanyuma ukangure kugirango byose bishonga kugirango ubone igisubizo kitagira ibara, hanyuma ushyiremo hydrati ya sodium ya 25.5 g, ugumane ubushyuhe kuri 80 ℃ hanyuma ugaruke kuri Iminota 15 kugirango ubone fordehide oxyde (10%) igisubizo kitagira ibara.

Muri ml 50 ya beaker, ongeramo 3,5 g p-aminobenzaldehyde, amazi 10 ml, ugabanye aside 5 ya hydrochloric aside, hanyuma ukomeze.Ibintu byumuhondo byoroheje bihinduka umukara vuba kandi bigashonga ubudahwema.Irashobora gushyuha neza (munsi ya 6 ℃) kugirango iseshe byose.Gira ubukonje mu bwogero bwumunyu, kandi ubushyuhe bugabanuka munsi ya 5 ℃.Muri iki gihe, p-aminobenzaldehyde hydrochloride igwa nkibice byiza, kandi igisubizo kiba paste.Mugihe cyo gukurura, 5-10 ℃ 5 ml ya sodium nitrite yumuti yatonywe muminota 20, hanyuma kubyutsa bikomeza kuminota 20.40% ya sodium acetate yakoreshejwe muguhindura impapuro zitukura za congo kugirango zidafite aho zibogamiye kugirango zibone igisubizo cyumunyu wa diazonium.

Kunyunyuza 0,7 g ya sulfate y'umuringa wa kristaline, 0,2 g ya sodium sulfite na 1,6 g ya sodium acetate ya hydrata mo 10% ya forode ya forode ya forode, hanyuma igisubizo gihinduka icyatsi.Nyuma yo gutonyanga, komeza ubushyuhe buke muminota 30 kugirango ubone igisubizo cyumuhondo, ongeramo ml 30 yibanze ya acide hydrochloric, uzamure ubushyuhe kuri 100 ℃, refluxe kumasaha 1, igisubizo kigaragara nkicunga, kuvanga amavuta, kubona umweru wera gato, kuyungurura no gukama kugirango ubone ibicuruzwa bya p-benzaldehyde.Igicuruzwa cyongeye gushyirwamo imbaraga zivanze na 1: 1 inzoga namazi.