1,4-Phthalaldehyde

Tāpirihia te 6.0 g o te konutai sulfide, 2.7 g o te paura whanariki, 5 g o te konutai waikawa me te 60 ml o te wai ki roto i te 250 ml o te ipu kaki e toru me te condenser reflux me te taputapu whakaoho, me te whakanui i te pāmahana ki te 80 ℃ i raro i te whakaoho.Ka memeha te paura whanariki Kōwhai, ka whero te otinga.Whai muri i te whakamaarama mo te 1 haora, ka whiwhi te otinga konutai polysulfide whero pouri.

Tāpirihia te 13.7 g o te p-nitrotoluene, 80 ml o te waihano ahumahi, 0.279 g o te N, N-dimethylformamide me te 2.0 g o te Urea ki roto i te 250 ml e toru nga pounamu kaki me te kohanga whakaheke, he rewharewha rewharewha me te taputapu whakaoho, wera me te whakaoho. ki te whakakore i te p-nitrotoluene kia whiwhi ai i te otinga kowhai marama.Ka piki haere te pāmahana ki te 80 ℃ ka noho tonu, ka whakahekehia te otinga konutai polysulfide kua oti te whakarite i runga ake nei, ka tere ka huri te wairewa ki te kahurangi, ka huri te kaariki pouri ki te parauri pouri, ka mutu ka huri ki te whero.Ka makahia i roto i te 1.5-2.0 haora, katahi ka pupuri i te 80 ℃ mo te whakahoki mai mo te 2 haora.Ka tere te mahi whakamaarama mamaoa.I te wa ano o te whakamaarama, ka taapirihia te 100 ml wai, ka kohia te 150 ml o te distillate, a ko te uara pH ko te 7. Ko te toenga o te wai ka whakamatao ki te huka kia tere ai te whakaheke i nga tioata kowhai marama, ka tangohia me te ether (30 ml × 5). ), ka whakaeto ka whakamaroke ki te whiwhi p-aminobenzaldehyde totoka kowhai.

Tāpirihia te 5.89 paraformaldehyde, 13.2 g hydroxylamine hydrochloride me te 85 ml wai ki roto i te 250 ml e toru nga ipu kaki, whakamahana me te whakaoho kia memeha katoa kia whiwhi ai i te wairewa kore tae, katahi ka tapirihia te 25.5 g konutai acetate hydrate, kia mau te pāmahana ki te 80 ℃ me te reflux mo 15 min ki te tiki formaldehyde oxime (10%) wairewa kore tae.

I roto i te ipurau 50 ml, tāpirihia te 3.5 g p-aminobenzaldehyde, 10 ml wai, maturuturu 5 ml waikawa pūmāota pūmāota, me te whakaoho tonu.Ka tere te pango o te matū kōwhai marama, ka memeha haere tonu.Ka taea te whakamahana tika (i raro iho i te 6 ℃) kia memeha katoa.Whakamaohia ki roto i te pati hukapapa tote, ka heke te pāmahana ki raro i te 5 ℃.I tenei wa, ka pupuhi te p-aminobenzaldehyde hydrochloride hei matūriki pai, ka waiho te otinga hei whakapiri.I raro i te whakakorikori, 5-10 ℃ 5 ml o te wairewa konutai nitrite i maturuturu i roto i te 20 meneti, ka haere tonu te whakaoho mo te 20 meneti.40% te wairewa konutai acetate i whakamahia hei whakatika i te pepa whakamatautau whero o Congo kia noho koretake kia whiwhi wairewa tote diazonium.

Whakarewahia te 0.7 kara o te konupora konukawata, 0.2 g o te konutai sulfite me te 1.6 g o te konutai acetate hydrate ki roto i te wairewa oxime formaldehyde 10%, ka huri kakariki te otinga.I muri i te pupuhi, kia mau ki te iti o te pāmahana mo te 30 min ki te tiki i te otinga hina, tāpiri 30 ml waikawa pūmāota pūmāota, whakaara i te pāmahana ki te 100 ℃, refluxe mo te 1 haora, te otinga puta karaka, mamaoa Māturu, tiki he ma paku kōwhai totoka, tātari me te whakamaroke ki te tiki i te hua parakore o te p-benzaldehyde.I rerystallized te hua ki te whakarewa whakauru o te 1:1 waipiro me te wai.