Methanol → HCID 20375085, compound

HRID 1449080Notes

Reaction equation

HRID 1449080 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][S:32]([CH3:35])(=[O:34])=[O:33])OCC)C>C(O)(=O)C>[CH2:3]([N:5]([CH2:8][CH3:9])[CH2:6][CH3:7])[CH3:4].[CH3:35][S: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:34])=[O:33]

Participants

6

Reactant 4

HCID 887MethanolHCID 8471TriethylamineHCID 668254-Hydrazinobenzenesulfonic acidHCID 57009956HCID 57009956, compound

Product 1

HCID 20375085HCID 20375085, 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 was added 23.5 g of ethylβ-methanesulfonylamino-β-ethoxyacrylate. The resulting solution was allowed to stand at room temperature for one week. The crystals precipitated were collected and recrystallized from methanol; thus 29 g of plate-like crystals of the objective compound of a melting point of 236° to 238° C. was obtained.

Workup

  1. waitto stand at room temperature for one week
  2. customThe crystals precipitated
  3. customwere collected
  4. customrecrystallized from methanol
  5. customthus 29 g of plate-like crystals of the objective compound of a melting point of 236° to 238° C. was obtained

Sources & evidence

ORD record
ord-5ef380bd2af54595b231ad1c1822d344
Source dataset
uspto-grants-1980_02
Patent number
US04188489

Reaction notes

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