Reaktion #965196

ord-fa02986f556c465589f7a0a62ccbc8be

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.WAITleft
  2. 2
    SonstigeAfter the completion of reaction
  3. 3
    Filtrationthe reaction mixture was filtered
  4. 4
    Sonstigethe filtrate was evaporated in vacuo
  5. 5
    FiltrationThe crude filter cake
  6. 6
    Waschenwas washed with n-hexane

Vorschrift

To a solution of pyridin-3-ylamine (20 g, 212.49 mmol, CAS RN 462-08-8) in a mixture of THF:Et2O (175 mL; 2.5:1 v/v) was added slowly a solution of pivaloyl chloride (26 mL, 212.5 mmol, CAS RN 3282-30-2) in THF (50 mL) and Et3N (44 mL, 318.7 mmol) at 0° C. and left stirring at that temperature for 1 h. After the completion of reaction, the reaction mixture was filtered, and the filtrate was evaporated in vacuo. The crude filter cake was washed with n-hexane to yield the title compound. Colorless crystalline solid (32 g, 85%). MS (ESI): m/z=179.4 [M+H]+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08987307B2uspto-grants-2015_03