Sodium Hydroxide → HCID 178508993, Verbindung

HRID 1396733Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1396733
Cl.[NH2:2][C:3]1[N:8]=[C:7]([OH:9])[C:6]([NH2:10])=[C:5]([OH:11])[N:4]=1.[OH-].[Na+].[S:14]1[CH:18]=[CH:17][CH:16]=[C:15]1[CH2:19][CH2:20][C:21](Cl)=[O:22].S1C=CC=C1CCC(O)=O>S(Cl)(Cl)=O.O>[NH2:2][C:3]1[N:8]=[C:7]([OH:9])[C:6]([NH:10][C:21](=[O:22])[CH2:20][CH2:19][C:15]2[S:14][CH:18]=[CH:17][CH:16]=2)=[C:5]([OH:11])[N:4]=1

Komponenten

7

Edukt 4

HCID 14798Sodium HydroxideHCID 7031693-(2-Thienyl)propanoic acidHCID 149601613-(2-Thienyl)-propanoic acid chlorideHCID 178479162HCID 178479162, Verbindung

Produkt 1

HCID 178508993HCID 178508993, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 24386Thionyl ChlorideLösungsmittel2×

Versuchsvorschrift

To a solution of 2,5-diaminopyrimidine-4,6-diol hydrogen chloride (1.04 g, 5.8 mmol) in sodium hydroxide (17.8 mmol) solution (25 ml of H2O) was added 3-thiophen-2-ylpropionyl chloride (6.4 mmol). The latter was prepared by refluxing 3-thiophen-2-ylpropionic acid (6.4 mmol) in thionyl chloride (500 μL) for 1 hour whereupon the excess of thionyl chloride was removed by evaporation in vacuo. The reaction mixture was stirred at room temperature for 18 hours. The pH of the suspension was adjusted to approximately 6 and the solids were filtered off. The title compound (1.25 g) was characterized by its mass spectrum: MS m/z (%): 515 ([M+H]+, 100).

Aufarbeitung

  1. customThe latter was prepared
  2. customwas removed by evaporation in vacuo
  3. filtrationthe solids were filtered off

Quellen und Nachweise

ORD-Eintrag
ord-d019bfbdc4f74bf487a8c48bd3608715
Quelldatensatz
uspto-grants-2014_12
Patentnummer
US08901132B2

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