Sodium Bicarbonate → HCID 69810477, Verbindung

HRID 1891238

Reaktionsgleichung

Reaktionsgleichung von HRID 1891238
[Si:1]([O:8][CH2:9][C:10]1[CH:11]=[C:12]([C:16]2[CH:17]=[CH:18][C:19]([NH2:22])=[N:20][CH:21]=2)[CH:13]=[CH:14][CH:15]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].C(=O)([O-])O.[Na+].Br[CH:29]([CH3:40])[C:30]([C:32]1[CH:37]=[CH:36][C:35]([F:38])=[CH:34][C:33]=1[F:39])=O>C(O)C>[Si:1]([O:8][CH2:9][C:10]1[CH:11]=[C:12]([C:16]2[CH:17]=[CH:18][C:19]3[N:20]([C:29]([CH3:40])=[C:30]([C:32]4[CH:37]=[CH:36][C:35]([F:38])=[CH:34][C:33]=4[F:39])[N:22]=3)[CH:21]=2)[CH:13]=[CH:14][CH:15]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]

Komponenten

5

Edukt 3

HCID 516892Sodium BicarbonateHCID 110758302-Bromo-1-(2,4-difluorophenyl)propan-1-oneHCID 44232378HCID 44232378, Verbindung

Produkt 1

HCID 69810477HCID 69810477, VerbindungAusbeute 49,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

300 mg of 5-[3-(tert-butyldimethylsilanyloxymethyl)phenyl]pyridin-2-ylamine dissolved in 5 ml of ethanol are placed in a screw reactor. 200 mg of sodium hydrogen carbonate and 470 mg of 2-bromo-1-(2,4-difluorophenyl)propan-1-one are added thereto. The reactor is closed and heated at 80° C. for 20 h. After cooling, the reaction mixture is concentrated under reduced pressure. The residue obtained is purified by silica gel chromatography, elution being carried out with a heptane/ethyl acetate mixture. 220 mg of compound are obtained.

Aufarbeitung

  1. customare placed in a screw reactor
  2. customThe reactor is closed
  3. temperatureAfter cooling
  4. concentrationthe reaction mixture is concentrated under reduced pressure
  5. customThe residue obtained
  6. customis purified by silica gel chromatography, elution

Quellen und Nachweise

ORD-Eintrag
ord-4fec0477d0454ff7882f382327028793
Quelldatensatz
uspto-grants-2013_08
Patentnummer
US08507520B2

Verknüpfte Notizen

Wird geladen…