2-bromo-N,N-diethylacetamide → HCID 135828231, Verbindung

HRID 720450Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 720450
[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.[CH2:20]([N:22]([CH2:27][CH3:28])[C:23](=[O:26])[CH2:24]Br)[CH3:21].C([O-])(O)=O.[Na+].C(Cl)Cl.CO>CN(C=O)C.O.C(OCC)(=O)C>[NH2:1][C:2]1[N:3]=[C:4]([S:19][CH2:24][C:23]([N:22]([CH2:27][CH3:28])[CH2:20][CH3:21])=[O:26])[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 2255452-bromo-N,N-diethylacetamideHCID 516892Sodium BicarbonateHCID 21226129Dichloromethane methanolHCID 178510481HCID 178510481, Verbindung

Produkt 1

HCID 135828231HCID 135828231, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

At RT, 53.6 mg (0.2 mmol) of 2-amino-4-(4-hydroxyphenyl)-6-sulfanyl-3,5-pyridinedicarbonitrile and 58.2 mg (0.3 mmol) of N,N-diethylbromoacetamide are stirred in 0.5 ml of DMF together with 33.6 mg (0.4 mmol) of NaHCO3 for 4 hours. TLC (CH2Cl2/CH3OH 10:1) shows complete conversion. The entire mixture is diluted with water and ethyl acetate 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-57c24c9c4d4b4f118c2b63c439fffa3e
Quelldatensatz
uspto-grants-2006_11
Patentnummer
US07135486B1

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