Reaktion #216908
ord-d9856abc93b2451cbf7466012acd1937
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturwas refluxed for 24 hours
- 2EinengenThe reaction mixture was concentrated under reduced pressure, isopropanol
- 3workup.ADDITIONwas added to the residue
- 4Filtrationthe resultant powder was collected by filtration
- 5workup.ADDITIONEthanol was added to the powder
- 6Filtrationthe insoluble matter was filtered off
- 7Einengenthe filtrate was concentrated to dryness
- 8workup.DISSOLUTIONThe residue was dissolved in water
- 9workup.ADDITIONadjusted to pH 6 by addition of diluted hydrochloric acid under ice cooling
- 10Filtrationthe resultant powder was collected by filtration
- 11Waschenwashed with ethanol
- 12Sonstigedried
Vorschrift
A mixture of 3.63 g of 3-acetylpyridine, 3.63 g of L-cysteine, 25 ml of water and 25 ml of ethanol was refluxed for 24 hours. The reaction mixture was concentrated under reduced pressure, isopropanol was added to the residue, and the resultant powder was collected by filtration. Ethanol was added to the powder, the insoluble matter was filtered off, and the filtrate was concentrated to dryness. The residue was dissolved in water and adjusted to pH 6 by addition of diluted hydrochloric acid under ice cooling and stirring, and the resultant powder was collected by filtration, washed with ethanol and dried to give 2.54 g of 2-methyl-2-(3-pyridyl)thiazolidine-4- carboxylic acid.