Reaktion #59236

ord-547275cf7a154823bb39f280951c9383

Reaktionsbedingungen

Temperatur
-5°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGThe resultant yellow colored solution was stirred at −5° C. for 1 h
  2. 2
    Sonstigethe solvents removed under reduced pressure
  3. 3
    workup.DISSOLUTIONthe resultant residue was dissolved in 1:1 v/v of ethyl acetate and water
  4. 4
    SonstigeThe organic layer was separated
  5. 5
    Waschenwashed with saturated solution of NaHCO3
  6. 6
    Trocknendried over Na2SO4
  7. 7
    SonstigeThe organic solvent was removed under reduced pressure
  8. 8
    Sonstigeto yield an orange colored solid
  9. 9
    SonstigeThe 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%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07425451B2uspto-grants-2008_09