Reaktion #163337

ord-392c23370f18485ea0366c42b5d658a8

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent is removed in vacuo
  2. 2
    SonstigeThe layers are separated
  3. 3
    Trocknenthe organic layer is dried with Na2SO4
  4. 4
    Filtrationfiltrated
  5. 5
    Sonstigethe solvent is removed in vacuo
  6. 6
    SonstigeThe crude product is purified by HPLC

Vorschrift

To 140 μl (1.68 mmol) 2-pyrrolidone in 5 mL DMF are added 110 mg (2.53 mmol) sodium hydride. Then 500 mg (1.68 mmol) 4-iodobenzyl bromide are added by several portions and the resulting mixture is stirred at r.t. over night. The solvent is removed in vacuo and the residue is resolved in DCM and water. The layers are separated and the organic layer is dried with Na2SO4, filtrated and the solvent is removed in vacuo. The crude product is purified by HPLC.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08835472B2uspto-grants-2014_09