Sulfuric Acid → HCID 178479471, Verbindung

HRID 1702608

Reaktionsgleichung

Reaktionsgleichung von HRID 1702608
[ClH:1].[NH:2]([CH2:6][C@H:7]1[CH2:12][CH2:11][C@H:10]([C:13]([OH:15])=[O:14])[CH2:9][CH2:8]1)[C:3]([NH2:5])=[NH:4].[CH:16]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH:19]=[CH:18][C:17]=1O.S(=O)(=O)(O)O.B(O)(O)O>CS(C)=O.C1(C)C(C)=CC=CC=1>[ClH:1].[NH:2]([CH2:6][C@H:7]1[CH2:12][CH2:11][C@H:10]([C:13]([O:15][C:18]2[CH:17]=[CH:16][C:25]3[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=3)[CH:19]=2)=[O:14])[CH2:9][CH2:8]1)[C:3]([NH2:5])=[NH:4]

Komponenten

7

Edukt 4

HCID 1118Sulfuric AcidHCID 7628Boric AcidHCID 86632-NaphtholHCID 178479474HCID 178479474, Verbindung

Produkt 1

HCID 178479471HCID 178479471, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 679Dimethyl SulfoxideLösungsmittelHCID 7237O-XyleneLösungsmittel

Versuchsvorschrift

A suspension of trans-4-guanidinomethylcyclohexanecarboxylic acid hydrochloride(1.8 g), β-naphtol(1.44 g), sulfuric acid(0.05 g) and boric acid(0.03 g) in a mixture of dimethylsulfoxide(10 ml) and xylene(50 ml) was heated under reflux conditions for 20 hours. The resulting water was removed by azeotropy with xylene. Following concentration of the reaction mixture, the residue was chromatographed on a column of silica gel with chloroform/methanol as eluent to give the title compound.

Aufarbeitung

  1. temperaturewas heated under reflux conditions for 20 hours
  2. customThe resulting water was removed by azeotropy with xylene
  3. customthe residue was chromatographed on a column of silica gel with chloroform/methanol as eluent

Quellen und Nachweise

ORD-Eintrag
ord-86b2ed1f7018499bbbc39add10230690
Quelldatensatz
uspto-grants-1982_09
Patentnummer
US04348410

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