1,4-Phthalaldehyde

Wedzera 6.0 g yesodium sulfide, 2.7 g yesulfur powder, 5 g yesodium hydroxide uye 60 ml yemvura mu 250 ml matatu mitsipa flask ine reflux condenser uye inobvongodza mudziyo, uye simudza tembiricha kusvika 80 ℃ pasi pekudzvinyirirwa.Iyo Yero sulfur poda inonyungudika, uye mhinduro inoshanduka tsvuku.Mushure mekudzokorora kwe1 h, yakasviba tsvuku sodium polysulfide mhinduro inowanikwa.

Wedzera 13.7 g yep-nitrotoluene, 80 ml ye ethanol yeindasitiri, 0,279 g yeN, N-dimethylformamide uye 2.0 g ye urea mu 250 ml matatu ane mitsipa flask ine funnel yekudonhedza, reflux condenser uye chinokuchidzira mudziyo, kupisa nekuzunguza. kunyungudutsa p-nitrotoluene kuwana mhinduro yeroro.Kana tembiricha ikasimudzwa zvishoma nezvishoma kusvika 80 ℃ uye ikachengetwa isingachinji, iyo sodium polysulfide mhinduro yakagadziridzwa munhanho iri pamusoro inodonhedzwa, uye mhinduro yacho inokurumidza kushanduka bhuruu, yobva yaita rima rakasvibira kuita dema dema, uye pakupedzisira rinoita tsvuku tsvuku.Iyo inodonhedzwa mukati meawa 1.5-2.0, uye yozochengetwa pa80 ℃ ye refluxing reaction kwemaawa maviri.Steam distillation inoitwa nekukurumidza.Panguva imwe chete ye distillation, 100 ml yemvura inowedzerwa, 150 ml ye distillate inounganidzwa, uye pH kukosha ndeye 7. Mvura yakasara inotonhodzwa nechando nokukurumidza kuti iwedzere chiedza chekrisiti yero, iyo inotorwa ne ether (30 ml × 5). ), yakavharwa uye yakaomeswa kuwana p-aminobenzaldehyde yero yakasimba.

Wedzera 5.89 paraformaldehyde, 13.2 g hydroxylamine hydrochloride uye 85 ml mvura mu 250 ml matatu ane mitsipa flask, kupisa uye kurunga kuti zvinyunguduke kuti zvinyunguduke kuwana mushonga usina ruvara, wobva wawedzera 25.5 g sodium acetate hydrate, chengetedza tembiricha iri pa80 ℃ uye reflux ye 15 min kuti uwane formaldehyde oxime (10%) isina ruvara mhinduro.

Mune 50 ml beaker, wedzera 3.5 g p-aminobenzaldehyde, 10 ml mvura, donhedza 5 ml concentrated hydrochloric acid, uye ramba uchikurudzira.Chinhu cheyero chakareruka chinoshanduka kuva dema nekukasira uye chinonyungudika chinoramba chiripo.Inogona kupiswa zvakanaka (pazasi pe6 ℃) kunyungudutsa yese.Itonhodze muchando chemunyu wekugezera, uye tembiricha inodonha kusvika pasi pe5 ℃.Panguva ino, p-aminobenzaldehyde hydrochloride inonaya sezvikamu zvakanaka, uye mhinduro yacho inonamira.Pasi pekusimudzira, 5-10 ℃ 5 ml ye sodium nitrite solution yakadonhedzwa mukati me20 min, uye kubvongodza kwakaenderera mberi kweinenge 20 min.40% sodium acetate solution yakashandiswa kugadzirisa iyo Congo red test bepa kuti ive isina kwayakarerekera kuwana diazonium munyu mhinduro.

Dissolve 0.7 g yecrystalline copper sulfate, 0.2 g ye sodium sulfite uye 1.6 g ye sodium acetate hydrate mu 10% formaldehyde oxime mhinduro, uye mhinduro inoshanduka yakasvibira.Mushure mekudonha, chengetedza yakaderera tembiricha kwemaminetsi makumi matatu kuti uwane grey solution, wedzera 30 ml concentrated hydrochloric acid, simudza tembiricha kusvika 100 ℃, refluxe kweawa imwe, mhinduro inoratidzika orenji, dhizaini yemhepo, tora chena zvishoma yellow solid, sefa uye woomesa kuti utore crude product ye p-benzaldehyde.Chigadzirwa chacho chakadzokororwa neyakasanganiswa solvent ye1: 1 doro nemvura.