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Hydrochloric Acid → HCID 54160621, Verbindung

HRID 648595
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 648595
[CH3:1][NH:2][C:3]1[S:4][C:5]([C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)=[C:6]([CH:8]=O)[N:7]=1.Cl.[I-].C1([P+](C2C=CC=CC=2)(C2C=CC=CC=2)[CH2:25][C:26]2[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=2)C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+].Cl>O1CCCC1.O>[CH3:1][NH:2][C:3]1[S:4][C:5]([C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)=[C:6]([CH:8]=[CH:25][C:26]2[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=2)[N:7]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 20144978HCID 20144978, VerbindungHCID 86741343HCID 86741343, Verbindung

Produkt 1

HCID 54160621HCID 54160621, VerbindungAusbeute 10,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962
Water
Lösungsmittel
HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 2-methylamino-4-formyl-5-(4-pyridyl)thiazole (1.1 g) in a mixture of tetrahydrofuran (40 ml) and water (40 ml) was added triphenyl (4-pyridylmethyl)phosphonium iodide hydrochloride (7.8 g). The resultant mixture was stirred at ambient temperature for 3 hours, during which time the mixture was maintained at pH 9.5 to 10 with 20% aqueous potassium carbonate. The reaction mixture was adjusted to pH 1.0 with 10% hydrochloric acid and washed with ethyl acetate. The aqueous solution was adjusted to pH 7.0 with 20% aqueous potassium carbonate and extracted with a mixture of ethyl acetate and tetrahydrofuran. The organic extract was dried over magnesium sulfate and evaporated in vacuo. The residue was subjected to column chromatography on silica gel eluting with a mixture of ethyl acetate and tetrahydrofuran (4:1). The fractions containing the desired compound were combined and evaporated in vacuo to give 2-methylamino-4-[2-(4-pyridyl)vinyl]-5-(4-pyridyl)thiazole (0.16 g).

Aufarbeitung

  1. washwashed with ethyl acetate
  2. extractionextracted with a mixture of ethyl acetate and tetrahydrofuran
  3. extractionThe organic extract
  4. dry with materialwas dried over magnesium sulfate
  5. customevaporated in vacuo
  6. additionThe residue was subjected to column chromatography on silica gel eluting with a mixture of ethyl acetate and tetrahydrofuran (4:1)
  7. additionThe fractions containing the desired compound
  8. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-051b856c9ca449d78c504b60dc1807d8
Quelldatensatz
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04735957

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