Sodium Bicarbonate → HCID 135828236, Verbindung

HRID 720449Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 720449
[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[C:6]([C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)[C:5]([C:17]#[N:18])=[C:4]([SH:19])[N:3]=1.[CH3:20][NH:21][C:22](=[O:25])[CH2:23]Br.C([O-])(O)=O.[Na+].C(Cl)Cl.CO>CN(C)C=O.O.C(OCC)(=O)C>[NH2:1][C:2]1[N:3]=[C:4]([S:19][CH2:23][C:22]([NH:21][CH3:20])=[O:25])[C:5]([C:17]#[N:18])=[C:6]([C:10]2[CH:11]=[CH:12][C:13]([OH:16])=[CH:14][CH:15]=2)[C:7]=1[C:8]#[N:9]

Komponenten

8

Edukt 4

HCID 516892Sodium BicarbonateHCID 154907452-Bromo-N-methylacetamideHCID 21226129Dichloromethane methanolHCID 178510481HCID 178510481, Verbindung

Produkt 1

HCID 135828236HCID 135828236, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

At room temperature (RT), 53.6 mg (0.2 mmol) of 2-amino-4-(4-hydroxyphenyl)-6-sulfanyl-3,5-pyridinedicarbonitrile and 45.6 mg (0.3 mmol) of N-methylbromoacetamide are stirred in 0.5 ml of dimethylformamide (DMF) together with 33.6 mg (0.4 mmol) of NaHCO3 for 4 hours. Thin-layer chromatography (TLC) (CH2Cl2/CH3OH 10:1) shows complete conversion. The entire mixture is diluted with water and ethyl acetate (EA) and the EA phase is dried with MgSO4 and concentrated under reduced pressure. The residue crystallizes from methanol.

Aufarbeitung

  1. dry with materialthe EA phase is dried with MgSO4
  2. concentrationconcentrated under reduced pressure
  3. customThe residue crystallizes from methanol

Quellen und Nachweise

ORD-Eintrag
ord-0cedceb4c08f46e5bdf40a55b4b3159f
Quelldatensatz
uspto-grants-2006_11
Patentnummer
US07135486B1

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