Reaktion #59236
ord-547275cf7a154823bb39f280951c9383
Reaktionsgleichung
Reagenzien
Reaktionsbedingungen
Aufarbeitung
- 1workup.STIRRINGThe resultant yellow colored solution was stirred at −5° C. for 1 h
- 2Sonstigethe solvents removed under reduced pressure
- 3workup.DISSOLUTIONthe resultant residue was dissolved in 1:1 v/v of ethyl acetate and water
- 4SonstigeThe organic layer was separated
- 5Waschenwashed with saturated solution of NaHCO3
- 6Trocknendried over Na2SO4
- 7SonstigeThe organic solvent was removed under reduced pressure
- 8Sonstigeto yield an orange colored solid
- 9SonstigeThe solid was triturated with hexane
Vorschrift
2,4,6-Trichloro-s-triazine (1, 1 g, 5.4 mmol), and ethylamine hydrochloride (0.44 g, 5.4 mmol) were combined in a round bottom flask and cooled to −5° C. using an ice-salt bath. To the cooled, stirred solution was added N,N-diisopropylethylamine (1.88 mL, 10.8 mmol). The resultant yellow colored solution was stirred at −5° C. for 1 h, the solvents removed under reduced pressure, and the resultant residue was dissolved in 1:1 v/v of ethyl acetate and water. The organic layer was separated, washed with saturated solution of NaHCO3, and dried over Na2SO4. The organic solvent was removed under reduced pressure to yield an orange colored solid. The solid was triturated with hexane to yield the product 2 as a yellow-orange powder (0.7 g) with a yield of 68%.