1,4-Phthaaldehyde 1

Ntxiv 6.0 g ntawm sodium sulfide, 2.7 g ntawm sulfur hmoov, 5 g ntawm sodium hydroxide thiab 60 ml ntawm dej rau hauv 250 ml peb necked hwj nrog reflux condenser thiab nplawm ntaus ntawv, thiab nce qhov kub ntawm 80 ℃ nyob rau hauv stirring.Yellow sulfur hmoov dissolves, thiab cov tshuaj hloov liab.Tom qab refluxing rau 1 h, tsaus liab sodium polysulfide tov yog tau.

Ntxiv 13.7 g ntawm p-nitrotoluene, 80 ml ntawm industrial ethanol, 0.279 g ntawm N, N-dimethylformamide thiab 2.0 g ntawm urea rau hauv 250 ml peb necked hwj nrog ib tug xa me nyuam rov funnel, reflux condenser thiab ib tug stirring ntaus ntawv, cua sov thiab do. kom yaj p-nitrotoluene kom tau lub teeb daj.Thaum qhov kub thiab txias tau maj mam nce mus txog 80 ℃ thiab khaws cia tas mus li, cov tshuaj sodium polysulfide npaj rau hauv cov kauj ruam saum toj no poob, thiab cov tshuaj sai sai tig xiav, tom qab ntawd hloov xim ntsuab mus rau xim av tsaus, thiab thaum kawg hloov xim av.Nws poob hauv 1.5-2.0 teev, thiab tom qab ntawd khaws cia ntawm 80 ℃ rau refluxing cov tshuaj tiv thaiv rau 2 teev.Chav distillation yog nqa tawm sai heev.Nyob rau tib lub sij hawm ntawm distillation, 100 ml dej yog ntxiv, 150 ml ntawm distillate yog sau, thiab pH nqi yog 7. Cov residual kua yog txias nrog dej khov sai sai rau precipitate lub teeb daj muaju, uas yog muab rho tawm nrog ether (30 ml × 5. ), evaporated thiab qhuav kom tau txais p-aminobenzaldehyde daj khoom.

Ntxiv 5.89 paraformaldehyde, 13.2 g hydroxylamine hydrochloride thiab 85 ml dej rau hauv 250 ml peb caj dab, cua sov thiab do kom lawv tag nrho yaj kom tau cov xim tsis muaj xim, ces ntxiv 25.5 g sodium acetate hydrate, kom kub ntawm 80 ℃ thiab reflux rau. 15 feeb kom tau txais formaldehyde oxime (10%) cov tshuaj tsis muaj xim.

Nyob rau hauv 50 ml beaker, ntxiv 3.5 g p-aminobenzaldehyde, 10 ml dej, poob 5 ml concentrated hydrochloric acid, thiab stirring tas li.Lub teeb daj cov khoom tig dub sai sai thiab dissolves tsis tu ncua.Nws tuaj yeem ua kom sov zoo (hauv qab 6 ℃) kom yaj tag nrho nws.Txias nws hauv dej khov ntsev da dej, thiab qhov kub poob qis dua 5 ℃.Lub sijhawm no, p-aminobenzaldehyde hydrochloride precipitates raws li cov khoom zoo, thiab cov tshuaj yuav muab tshuaj txhuam.Nyob rau hauv stirring, 5-10 ℃ 5 ml ntawm sodium nitrite tov yog dripped nyob rau hauv 20 min, thiab stirring yog txuas ntxiv rau li 20 min.40% sodium acetate tov tau siv los kho Congo liab daim ntawv xeem kom nruab nrab kom tau txais diazonium ntsev tov.

Dissolve 0.7 g ntawm crystalline tooj liab sulfate, 0.2 g ntawm sodium sulfite thiab 1.6 g ntawm sodium acetate hydrate rau hauv 10% formaldehyde oxime tov, thiab cov tshuaj hloov ntsuab.Tom qab dripping, cia qhov kub thiab txias rau 30 feeb kom tau txais cov tshuaj grey, ntxiv 30 ml concentrated hydrochloric acid, nce qhov kub thiab txias rau 100 ℃, refluxe rau 1 teev, cov tshuaj zoo li txiv kab ntxwv, chav distillation, tau ib tug dawb me ntsis daj khoom, lim thiab qhuav kom tau cov khoom nyoos ntawm p-benzaldehyde.Cov khoom yog recrystallized nrog tov hnyav ntawm 1: 1 cawv thiab dej.