Hydrochloric Acid → 3-Morpholino-1-(p-sulfophenyl)-5-pyrazolone Triethylamine Salt

HRID 1449078

反応式

HRID 1449078 の反応式
C(O)C.[O:4]1[CH2:9][CH2:8][N:7]([C:10](OCC)=[CH:11][C:12](N2CCOCC2)=[O:13])[CH2:6][CH2:5]1.[S:23]([C:27]1[CH:32]=[CH:31][C:30]([NH:33][NH2:34])=[CH:29][CH:28]=1)([OH:26])(=[O:25])=[O:24].Cl>C(N(CC)CC)C.C(O)(C)C.C(O)(=O)C>[CH2:6]([N:7]([CH2:10][CH3:11])[CH2:8][CH3:9])[CH3:5].[O:4]1[CH2:9][CH2:8][N:7]([C:10]2[NH:34][N:33]([C:30]3[CH:29]=[CH:28][C:27]([S:23]([OH:26])(=[O:24])=[O:25])=[CH:32][CH:31]=3)[C:12](=[O:13])[CH:11]=2)[CH2:6][CH2:5]1

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 668254-Hydrazinobenzenesulfonic acidHCID 53820735beta-Morpholino-beta-ethoxy-acrylic morpholide

生成物 1

HCID 203750883-Morpholino-1-(p-sulfophenyl)-5-pyrazolone Triethylamine Salt

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 3776Isopropanol溶媒HCID 8471Triethylamine溶媒

実験手順

Into 70 ml of ethanol was dissolved 13.5 g of β-morpholino-β-ethoxy-acrylic morpholide, and 9.4 g of p-sulfophenyl hydrazine was dissolved in a mixed solution of 30 g of triethylamine and 18 g of glacial acetic acid. The two solutions were then mixed. The resulting mixed solution was boiled on a steam bath for 8 hours. The mixture was then concentrated under reduced pressure to thereby provide a reddish, oily compound, to which 50 ml of isopropyl alcohol and 10 ml of concentrated hydrochloric acid (38 wt%) were added. Upon standing the thus obtained solution in a refrigerator for one night, crystals precipitated. The crystals were collected and recrystallized from ethanol, whereupon 9.8 g of crystals of the objective compound of a melting point of 203° to 205° C. was obtained.

後処理

  1. additionThe two solutions were then mixed
  2. additionThe resulting mixed solution
  3. concentrationThe mixture was then concentrated under reduced pressure
  4. customto thereby provide a reddish, oily compound
  5. customfor one night
  6. customcrystals precipitated
  7. customThe crystals were collected
  8. customrecrystallized from ethanol, whereupon 9.8 g of crystals of the objective compound of a melting point of 203° to 205° C.
  9. customwas obtained

出典と根拠

ORDレコード
ord-6497268f89704c078b81e569a6af86cc
出典データセット
uspto-grants-1980_02
特許番号
US04188489

関連ノート

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