Methanol → HCID 20375076, compound

HRID 1449079Notes

Reaction equation

HRID 1449079 reaction equation
CO.[CH2:3]([N:5]([CH2:8][CH3:9])[CH2:6][CH3:7])[CH3:4].[S:10]([C:14]1[CH:19]=[CH:18][C:17]([NH:20][NH2:21])=[CH:16][CH:15]=1)([OH:13])(=[O:12])=[O:11].C([O:24][C:25](=O)[CH:26]=[C:27]([NH:31][C:32](=[O:39])[C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)OCC)C>C(O)(=O)C>[CH2:3]([N:5]([CH2:8][CH3:9])[CH2:6][CH3:7])[CH3:4].[C:32]([NH:31][C:27]1[NH:21][N:20]([C:17]2[CH:16]=[CH:15][C:14]([S:10]([OH:13])(=[O:11])=[O:12])=[CH:19][CH:18]=2)[C:25](=[O:24])[CH:26]=1)(=[O:39])[C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1

Participants

6

Reactant 4

HCID 887MethanolHCID 8471TriethylamineHCID 668254-Hydrazinobenzenesulfonic acidHCID 53844518HCID 53844518, compound

Product 1

HCID 20375076HCID 20375076, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

Into a mixed solution of 50 ml of methanol, 50 ml of triethylamine and 50 ml of glacial acetic acid there was dissolved 18.8 g of p-sulfophenyl hydrazine, to which 26.3 g of ethylβ-benzoylamino-β-ethoxyacrylate was then added. The resulting solution was allowed to stand at room temperature for one week. The crystals which precipitated were collected and recrystallized from methanol; thus, 32 g of pale yellow crystals of the objective compound of a melting point of 275° to 278° C. was obtained.

Workup

  1. waitto stand at room temperature for one week
  2. customThe crystals which precipitated
  3. customwere collected
  4. customrecrystallized from methanol

Sources & evidence

ORD record
ord-0cd054b3007344889403e8738e53375a
Source dataset
uspto-grants-1980_02
Patent number
US04188489

Reaction notes

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