Lawesson's reagent → HCID 59176770, Verbindung

HRID 215968Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 215968
[C:1]1([CH2:11][CH:12]2[N:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]3=[N:14][C:13]2=O)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:31]2)=CC=1>C1(C)C=CC=CC=1.CO>[C:1]1([CH2:11][CH:12]2[N:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]3=[N:14][C:13]2=[S:31])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

Komponenten

5

Edukt 2

HCID 87949Lawesson's reagentHCID 59176789HCID 59176789, Verbindung

Produkt 1

HCID 59176770HCID 59176770, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
160 °C

Versuchsvorschrift

A suspension of 200 mg (0.73 mmol) of 3-naphthalen-1-ylmethyl-imidazo[1,2-a]pyridin-2-one and 250 mg (0.62 mmol) of 2,4-bis-(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane 2,4-disulfide (Lawesson's reagent) in 20 mL of toluene is heated at 160° C. for 1 h under microwave condition. The resulting mixture is dissolved in methanol and absorbed on silica gel. The slurry is dried under reduced pressure and is purified by flash chromatography on silica gel. The compound is eluted 5˜10% methanol in dichloromethane solution to give the desired compound.

Aufarbeitung

  1. customabsorbed on silica gel
  2. customThe slurry is dried under reduced pressure
  3. customis purified by flash chromatography on silica gel
  4. washThe compound is eluted 5˜10% methanol in dichloromethane solution

Quellen und Nachweise

ORD-Eintrag
ord-4afb7a9cdde94e8aafa4522f74e0360b
Quelldatensatz
uspto-grants-2012_06
Patentnummer
US08193214B2

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