Acetonitrile → 3-Phenylureido-1-(p-sulfophenyl)-5-pyrazolone Triethylamine Salt

HRID 1449075

반응식

HRID 1449075 반응식
[C:1](#[N:3])[CH3:2].[C:4](OOC(CC)(N)C)(=[O:7])[CH:5]=C.[C:15]1([N:21]=[C:22]=[O:23])[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[S:24]([C:28]1[CH:33]=[CH:32][C:31]([NH:34][NH2:35])=[CH:30][CH:29]=1)([OH:27])(=[O:26])=[O:25]>C(O)(=O)C.C(N(CC)CC)C.CO>[CH2:1]([N:3]([CH2:15][CH3:16])[CH2:4][CH3:5])[CH3:2].[C:15]1([NH:21][C:22](=[O:23])[NH:3][C:1]2[NH:35][N:34]([C:31]3[CH:30]=[CH:29][C:28]([S:24]([OH:27])(=[O:25])=[O:26])=[CH:33][CH:32]=3)[C:4](=[O:7])[CH:2]=2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

참가 물질

8

반응물 4

HCID 6342AcetonitrileHCID 7672Phenyl isocyanateHCID 668254-Hydrazinobenzenesulfonic acidHCID 86736826Ethylbeta-amino-beta-ethoxy acrylate

생성물 1

HCID 867368303-Phenylureido-1-(p-sulfophenyl)-5-pyrazolone Triethylamine Salt

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 887Methanol용매HCID 8471Triethylamine용매

실험 절차

Into 30 ml of acetonitrile was dissolved 4 g of ethylβ-amino-β-ethoxy acrylate, and 3 g of phenyl isocyanate was added thereto. The resulting solution was allowed to stand at room temperature for 24 hours. Into a mixed solution of 20 ml of methanol, 6 g of triethylamine and 5 ml of glacial acetic acid there was dissolved 4.7 g of p-sulfophenyl hydrazine, and the above solution, in which the esterification reaction had been completed, was added thereto. The resulting solution was allowed to stand at room temperature for 5 days. The crystals obtained were collected, washed with acetonitrile, and then recrystallized from methanol; thus 7.5 g of crystals of a melting point of 240° to 242° C. was obtained.

후처리

  1. additionwas added
  2. customthe above solution, in which the esterification reaction
  3. additionwas added
  4. waitto stand at room temperature for 5 days
  5. customThe crystals obtained
  6. customwere collected
  7. washwashed with acetonitrile
  8. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-8e38e84ac0384cd49f4bbe68de885163
출처 데이터셋
uspto-grants-1980_02
특허 번호
US04188489

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