HCID 15086004, Verbindung → HCID 21256462, Verbindung

HRID 635859Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 635859
[N:1]1[CH:2]=[C:3]([CH2:13][OH:14])[N:4]2[C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=3[S:6][C:5]=12>CN(C=O)C.C1(C)C=CC=CC=1.O=[Mn]=O>[N:1]1[CH:2]=[C:3]([CH:13]=[O:14])[N:4]2[C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=3[S:6][C:5]=12

Komponenten

5

Edukt 1

HCID 15086004HCID 15086004, Verbindung

Produkt 1

HCID 21256462HCID 21256462, VerbindungAusbeute 101 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 14801Manganese dioxideKatalysatorHCID 1140TolueneLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of imidazo[2,1-b]benzothiazole-3-methanol (Formula J-2) (2.0 g) in DMF (30 mL) and toluene (200 mL) was treated with MnO2 (4.5 g) and the mixture was azeotropically distilled for 4.5 hours. A second change of MnO2 (2.0 g) and distillation for 1 hour completed the conversion. The suspension was filtered, the combined filtrate and ethyl acetate washes of the cake were concentrated, the residue was diluted with water, and filtered to yield imidazo[2,1-b]benzothiazole-3-carboxaldehyde (Formula J-3) (2.0 g). Crude imidazo[2,1-b]benzothiazole-3-carboxaldehyde (Formula J-3) was used without further purification.

Aufarbeitung

  1. distillationthe mixture was azeotropically distilled for 4.5 hours
  2. distillationA second change of MnO2 (2.0 g) and distillation for 1 hour
  3. filtrationThe suspension was filtered
  4. concentrationthe combined filtrate and ethyl acetate washes of the cake were concentrated
  5. additionthe residue was diluted with water
  6. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-79aad8076cb54545a3b087e9f2968385
Quelldatensatz
uspto-grants-2001_02
Patentnummer
US06191124B1

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