Water → HCID 68034539, Verbindung

HRID 2408335

Reaktionsgleichung

Reaktionsgleichung von HRID 2408335
[Cl:1][C:2]1[N:3]=[C:4]2[NH:11][C:10]([CH3:13])([CH3:12])[CH2:9][N:5]2[C:6](=[O:8])[CH:7]=1.C(=O)([O-])[O-].[Cs+].[Cs+].CC1C=CC(S(O[CH2:31][CH2:32][O:33][CH:34]([CH3:36])[CH3:35])(=O)=O)=CC=1.O>CC#N.C(OCC)(=O)C>[Cl:1][C:2]1[N:3]=[C:4]2[N:11]([CH2:31][CH2:32][O:33][CH:34]([CH3:36])[CH3:35])[C:10]([CH3:13])([CH3:12])[CH2:9][N:5]2[C:6](=[O:8])[CH:7]=1

Komponenten

7

Edukt 4

HCID 962WaterHCID 10796Cesium carbonateHCID 19099443HCID 19099443, VerbindungHCID 1363591007-chloro-2,2-dimethyl-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one

Produkt 1

HCID 68034539HCID 68034539, VerbindungAusbeute 59,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6342AcetonitrileLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
65 °C

Versuchsvorschrift

To 0.200 g of 7-chloro-2,2-dimethyl-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one suspended in 7 mL of CH3CN, 0.65 g of cesium carbonate and 0.51 g of 2-isopropoxyethyl 4-methylbenzenesulfonate are added. The mixture is heated to 65° C. for 36 h. Water, ethyl acetate are added and then after decantation, the organic phase is dried with magnesium sulfate and then evaporated. The crude is purified by flash chromatography on silica gel (CH2Cl2/MeOH, 99/1). 0.17 g (yield=45%) of 7-chloro-1-(2-isopropoxyethyl)-2,2-dimethyl-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one are obtained as a brown powder.

Aufarbeitung

  1. dry with materialafter decantation, the organic phase is dried with magnesium sulfate
  2. customevaporated
  3. customThe crude is purified by flash chromatography on silica gel (CH2Cl2/MeOH, 99/1)

Quellen und Nachweise

ORD-Eintrag
ord-ccf501ae24a54f1397e08b43a7be80bf
Quelldatensatz
uspto-grants-2014_08
Patentnummer
US08815853B2

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