Ethanol → 3-Anilino-1-(p-sulfophenyl)-5-pyrazolone

HRID 1449076

반응식

HRID 1449076 반응식
[CH2:1]([OH:3])[CH3:2].C(OO[C:10](CC)([NH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)C)(=O)C=C.[S:21]([C:25]1[CH:30]=[CH:29][C:28]([NH:31][NH2:32])=[CH:27][CH:26]=1)([OH:24])(=[O:23])=[O:22].C(N(CC)CC)C>C(O)(=O)C>[NH:12]([C:10]1[NH:32][N:31]([C:28]2[CH:29]=[CH:30][C:25]([S:21]([OH:24])(=[O:22])=[O:23])=[CH:26][CH:27]=2)[C:1](=[O:3])[CH:2]=1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

참가 물질

6

반응물 4

HCID 702EthanolHCID 8471TriethylamineHCID 668254-Hydrazinobenzenesulfonic acidHCID 86736832Ethylbeta-anilino-beta-ethoxy acrylate

생성물 1

HCID 204789123-Anilino-1-(p-sulfophenyl)-5-pyrazolone

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Into 1.5 l of ethanol were dispersed 118 g of ethylβ-anilino-β-ethoxy acrylate and 94 g of p-sulfophenylhydrazine, and 150 g of triethylamine and glacial acetic acid were successively dropped thereinto while heating (95°-100° C.) and stirring. After heating (95°-100° C.) and stirring for 5 hours, the reaction solution was concentrated under reduced pressure. To the residue so concentrated were added 50 ml of water and 120 ml of ethanol containing 35% by wt. hydrogen chloride to provide a uniform solution. This uniform solution was allowed to stand in a refrigerator for one day and one night. The crystals of the objective compound which precipitated had a melting point of 290° to 291° C. and weighed 145 g.

후처리

  1. additionwere successively dropped
  2. temperaturewhile heating (95°-100° C.)
  3. temperatureAfter heating (95°-100° C.)
  4. stirringstirring for 5 hours
  5. concentrationthe reaction solution was concentrated under reduced pressure
  6. concentrationTo the residue so concentrated
  7. additionwere added 50 ml of water and 120 ml of ethanol containing 35% by wt. hydrogen chloride
  8. customto provide a uniform solution
  9. customThe crystals of the objective compound which precipitated

출처 및 근거

ORD 기록
ord-8f94abe7944a45dd8559084c155330ef
출처 데이터셋
uspto-grants-1980_02
특허 번호
US04188489

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