Sodium Bicarbonate → HCID 68638439, Verbindung

HRID 2196453Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2196453
Br[CH:2]([CH3:10])[C:3]([C:5]1[S:6][CH:7]=[CH:8][CH:9]=1)=O.C(=O)([O-])O.[Na+].[Si:16]([O:23][CH2:24][C:25]1[CH:26]=[C:27]([C:31]2[CH:32]=[CH:33][C:34]([NH2:37])=[N:35][CH:36]=2)[CH:28]=[CH:29][CH:30]=1)([C:19]([CH3:22])([CH3:21])[CH3:20])([CH3:18])[CH3:17]>C(O)C>[Si:16]([O:23][CH2:24][C:25]1[CH:26]=[C:27]([C:31]2[CH:32]=[CH:33][C:34]3[N:35]([C:2]([CH3:10])=[C:3]([C:5]4[S:6][CH:7]=[CH:8][CH:9]=4)[N:37]=3)[CH:36]=2)[CH:28]=[CH:29][CH:30]=1)([C:19]([CH3:22])([CH3:21])[CH3:20])([CH3:18])[CH3:17]

Komponenten

5

Edukt 3

HCID 516892Sodium BicarbonateHCID 117699522-Bromo-1-(thiophen-2-yl)propan-1-oneHCID 442323785-[3-(tert-Butyldimethylsilanyloxymethyl)phenyl]pyridin-2-ylamine

Produkt 1

HCID 68638439HCID 68638439, VerbindungAusbeute 67,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

In a glass tube, 280 mg of 5-[3-(tert-butyldimethylsilanyloxymethyl)phenyl]pyridin-2-ylamine, 390 mg of 2-bromo-1-thiophen-2-ylpropan-1-one and 190 mg of sodium hydrogencarbonate are dissolved in 5 ml of ethanol. The tube is closed and heated at 100° C. for 20 h. After cooling, the mixture is concentrated under reduced pressure. The residue is purified by silica gel chromatography, elution being carried out with a heptane/ethyl acetate mixture. 260 mg of compound are obtained.

Aufarbeitung

  1. customThe tube is closed
  2. temperatureAfter cooling
  3. concentrationthe mixture is concentrated under reduced pressure
  4. customThe residue is purified by silica gel chromatography, elution

Quellen und Nachweise

ORD-Eintrag
ord-74952a896aff4453826db99d96a0be16
Quelldatensatz
uspto-grants-2012_12
Patentnummer
US08338451B2

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