1,4-Phthalaldehyde

E hoʻohui i 6.0 g o ka sodium sulfide, 2.7 g o ka pauka sulfur, 5 g o ka sodium hydroxide a me 60 ml o ka wai i loko o ka 250 ml ʻekolu pahu ʻāʻī me ka reflux condenser a me ka mea hoʻouluulu, a hoʻonui i ka mahana i 80 ℃ ma lalo o ka hoʻoulu ʻana.Hoʻoheheʻe ʻia ka pauda sulfur melemele, a ʻulaʻula ka hopena.Ma hope o ka refluxing no 1 h, loaʻa ka ʻulaʻula ʻulaʻula sodium polysulfide solution.

E hoʻohui i 13.7 g o ka p-nitrotoluene, 80 ml o ka ethanol ʻoihana, 0.279 g o N, N-dimethylformamide a me 2.0 g o ka urea i loko o ka 250 ml ʻekolu ʻāʻī ʻāʻī me kahi funnel hāʻule, kahi reflux condenser a me kahi mea hoʻouluulu, wela a hoʻoulu. e hoʻoheheʻe i ka p-nitrotoluene e loaʻa ai kahi hopena melemele māmā.Ke hoʻokiʻekiʻe mālie ʻia ka mahana i 80 ℃ a mālama mau ʻia, hāʻule ka solution sodium polysulfide i hoʻomākaukau ʻia ma ka ʻanuʻu i luna, a huli koke ka hopena i polū, a laila lilo ka ʻōmaʻomaʻo ʻeleʻele i ʻeleʻele ʻeleʻele, a ʻo ka hope e lilo i ʻulaʻula ʻulaʻula.Hoʻokuʻu ʻia ia i loko o 1.5-2.0 mau hola, a laila mālama ʻia ma 80 ℃ no ka refluxing reaction no 2 mau hola.Hoʻokō koke ʻia ka distillation mahu.I ka manawa like o ka distillation, hoʻohui ʻia ka 100 ml wai, 150 ml o ka distillate e hōʻiliʻili ʻia, a ʻo ka pH waiwai ʻo 7. Hoʻomaʻalili ʻia ke koena wai me ka hau wikiwiki e hoʻoheheʻe i nā kristal melemele māmā, i unuhi ʻia me ka ether (30 ml × 5 ), hoʻoheheʻe ʻia a maloʻo no ka loaʻa ʻana o ka p-aminobenzaldehyde melemele paʻa.

E hoʻohui i ka 5.89 paraformaldehyde, 13.2 g hydroxylamine hydrochloride a me 85 ml wai i loko o ka 250 ml ʻekolu pahu ʻāʻī, wela a hoʻoulu e hoʻoheheʻe iā lākou a pau e loaʻa ai kahi hopena kala ʻole, a laila hoʻohui i ka 25.5 g sodium acetate hydrate, mālama i ka mahana ma 80 ℃ a reflux no ka 15 min no ka loaʻa ʻana o ka formaldehyde oxime (10%) kala ʻole.

I loko o kahi pahu wai 50 ml, e hoʻohui i 3.5 g p-aminobenzaldehyde, 10 ml wai, e hoʻokuʻu i 5 ml hydrochloric acid concentrated, a hoʻomau i ka hoʻoulu ʻana.ʻEleʻele koke ka mea melemele māmā a hoʻoheheʻe mau.Hiki ke hoʻomehana maikaʻi ʻia (ma lalo o 6 ℃) e hoʻoheheʻe i nā mea āpau.E hooluolu i loko o ka ʻauʻau paʻakai hau, a hāʻule ka mahana ma lalo o 5 ℃.I keia manawa, p-aminobenzaldehyde hydrochloride precipitates e like me ka maikai particles, a lilo ka hopena i paʻi.Ma lalo o ka hoʻoulu ʻana, 5-10 ℃ 5 ml o ka sodium nitrite solution i kulu ʻia i loko o 20 min, a hoʻomau ʻia ka hoʻoulu ʻana no kahi o 20 min.Ua hoʻohana ʻia ʻo 40% sodium acetate solution no ka hoʻoponopono ʻana i ka pepa hōʻike ʻulaʻula ʻo Congo i kū ʻole no ka loaʻa ʻana o ka paʻakai diazonium.

E hoʻoheheʻe i 0.7 g o ka crystalline copper sulfate, 0.2 g o ka sodium sulfite a me 1.6 g o ka sodium acetate hydrate i loko o 10% formaldehyde oxime solution, a huli ka ʻōmaʻomaʻo.Ma hope o ka kulu ʻana, e mālama i ka mahana haʻahaʻa no 30 min e loaʻa ai kahi hopena hina, hoʻohui i ka 30 ml hydrochloric acid concentrated, hoʻokiʻekiʻe i ka mahana i 100 ℃, refluxe no 1 hola, ʻike ʻia ka hopena i ka ʻalani, ka distillation mahu, e loaʻa i kahi keʻokeʻo melemele paʻa, kānana a hoʻomaloʻo no ka loaʻa ʻana o ka hua palaka o p-benzaldehyde.Hoʻopili hou ʻia ka huahana me ka solvent hui ʻia o ka waiʻona 1: 1 a me ka wai.