2-bromo-N-ethylacetamide → HCID 135828226, Verbindung

HRID 720451Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 720451
[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]([NH:22][C:23](=[O:26])[CH2:24]Br)[CH3:21].C([O-])(O)=O.[Na+]>CN(C=O)C>[NH2:1][C:2]1[N:3]=[C:4]([S:19][CH2:24][C:23]([NH:22][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

5

Edukt 3

HCID 2207922-bromo-N-ethylacetamideHCID 516892Sodium BicarbonateHCID 178510481HCID 178510481, Verbindung

Produkt 1

HCID 135828226HCID 135828226, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

At RT 0.76 g (2 mmol) of 2-amino-4-(4-hydroxyphenyl)-6-sulfanyl-3,5-pyridinedicarbonitrile and 0.5 g (3 mmol) of N-ethylbromoacetamide are stirred in 5 ml of DMF together with 0.34 g (4 mmol) of NaHCO3 for 4 hours. After dilution with water, the mixture is extracted with ethyl acetate and the ethyl acetate phase is dried with MgSO4 and concentrated under reduced pressure. The solid residue obtained after concentration is stirred with methanol. The crystals are filtered off with suction and dried under reduced pressure.

Aufarbeitung

  1. extractionAfter dilution with water, the mixture is extracted with ethyl acetate
  2. dry with materialthe ethyl acetate phase is dried with MgSO4
  3. concentrationconcentrated under reduced pressure
  4. customThe solid residue obtained
  5. concentrationafter concentration
  6. filtrationThe crystals are filtered off with suction
  7. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-7ac6ea661a9442ca9e2a1260ec8ddce6
Quelldatensatz
uspto-grants-2006_11
Patentnummer
US07135486B1

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