Reaktion #2180253
ord-2b6a36a2e8c0433680e5e0eb97cf45a2
Reaktionsgleichung
Edukte
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeReaction mixture
- 2Sonstigewas brought to room temperature
- 3SonstigeReaction mixture
- 4Einengenwas concentrated
- 5workup.ADDITIONdiluted with water
- 6Extraktionextracted dichloromethane
- 7Waschenwashed with brine solution
- 8Trocknendried over anhydrous Na2SO4
- 9EinengenConcentrated
- 10Sonstigepurified by column chromatography
Vorschrift
Triethyl amine (1.0 eq) was added to solution of N-(2-aminophenyl)-4,5,6,7-tetrahydro[1,3]thiazolo[5,4-c]pyridine-2-carboxamide obtained in step VIII of example I (1.0 mmol) in 10 mL THF. The solution was cooled to 0° C. 4-Methyl-benzenesulfonyl chloride (1.0 mmol) was added slowly with continuous stirring. Reaction mixture was brought to room temperature and stirred for 2 h Reaction mixture was concentrated, diluted with water, extracted dichloromethane, washed with brine solution, and dried over anhydrous Na2SO4. Concentrated and purified by column chromatography to yield the title compound.