Sulfuric Acid → HCID 178484896, Verbindung

HRID 851753Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 851753
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[CH:10][NH:11][CH:12]=2)=[CH:4][CH:3]=1.[CH2:13](OC(OCC)OCC)C.OS(O)(=O)=O.[CH3:28][NH2:29]>C(O)C.Cl>[CH3:28][NH:29][CH:13]=[N:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:9]=[CH:10][NH:11][CH:12]=2)=[CH:6][CH:7]=1

Komponenten

7

Edukt 4

HCID 1118Sulfuric AcidHCID 6329MethylamineHCID 31214Ethyl orthoformateHCID 178507418HCID 178507418, Verbindung

Produkt 1

HCID 178484896HCID 178484896, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittelHCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 1.59 gm of 4-(4-aminophenyl)-1-H-imidazole and 2.22 gm of triethylorthoformate was heated for 30 minutes at 100° C. in the presence of a catalytic amount of 96% H2SO4. A 33% solution of methylamine in ethanol (9.5 gm) was then added dropwise to the cooled reaction mixture. The solution was stirred at room temperature for twenty hours and then evaporated to dryness. The residue obtained was dissolved in 10% hydrochloric acid, and the acid solution was washed with ethyl acetate and then adjusted to pH 10 with 10% NaOH. The product which separated was extracted with ethyl acetate to yield, after evaporation of the solvent, 0.45 gm of the desired compound.

Aufarbeitung

  1. customevaporated to dryness
  2. customThe residue obtained
  3. washthe acid solution was washed with ethyl acetate
  4. customThe product which separated
  5. extractionwas extracted with ethyl acetate
  6. customto yield
  7. customafter evaporation of the solvent, 0.45 gm of the desired compound

Quellen und Nachweise

ORD-Eintrag
ord-eb4b2041fe6b48569ffc77bd240ee570
Quelldatensatz
uspto-grants-1983_05
Patentnummer
US04386099

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