HCID 21256450, Verbindung → 174209-00-8

HRID 635847Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 635847
[CH3:1][C:2]1[N:3]2[C:9]([CH2:10][OH:11])=[CH:8][N:7]=[C:4]2[S:5][CH:6]=1>CN(C=O)C.C1(C)C=CC=CC=1.O=[Mn]=O>[CH3:1][C:2]1[N:3]2[C:9]([CH:10]=[O:11])=[CH:8][N:7]=[C:4]2[S:5][CH:6]=1

Komponenten

5

Edukt 1

HCID 21256450HCID 21256450, Verbindung

Produkt 1

HCID 21256490174209-00-8Ausbeute 22,7 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 14801Manganese dioxideKatalysatorHCID 1140TolueneLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 3-Methylimidazo[2,1-b]thiazole-5-methanol (FIG. C-5) (0.9 g) in DMF (10 mL) was diluted with toluene (200 mL), treated with MnO2 (3.0), and azeotropically distilled for 1.5 hours. The suspension was filtered and the filtrate was concentrated to 10 mL. The concentrate was diluted with ice water and the precipitated 3-Methylimidazo[2,1-b]thiazole-5-carboxaldehyde (FIG. C-6) (0.665 g) was filtered. An aliquot (225 mg) was recrystallized from ethyl acetate-hexane to yield pure 3-Methylimidazo[2,1-b]thiazole-5-carboxaldehyde (FIG. C-6) (202 mg), m.p. 163-165°.

Aufarbeitung

  1. distillationazeotropically distilled for 1.5 hours
  2. filtrationThe suspension was filtered
  3. concentrationthe filtrate was concentrated to 10 mL
  4. additionThe concentrate was diluted with ice water
  5. filtrationthe precipitated 3-Methylimidazo[2,1-b]thiazole-5-carboxaldehyde (FIG. C-6) (0.665 g) was filtered
  6. customAn aliquot (225 mg) was recrystallized from ethyl acetate-hexane

Quellen und Nachweise

ORD-Eintrag
ord-1cfbedca2f9d430bab25174ce5e20675
Quelldatensatz
uspto-grants-2001_02
Patentnummer
US06191124B1

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