Reaktion #1858597

ord-5de70b8108b442bf833bba75367ebcb6

Lösungsmittel

Reaktionsbedingungen

Temperatur
120°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe mixture was degassed with N2
  2. 2
    EinengenThe reaction mixture was concentrated under vacuum
  3. 3
    Sonstigepurified by separation method K
  4. 4
    workup.ADDITIONK2CO3 was added to the reaction crude (in MeOH)

Vorschrift

To a degassed solution of 2-(5-bromoisochroman-1-yl)-4,5-dihydro-1H-imidazole (300 mg) in Et3N (10 ml) and ethynyltrimethylsilane (210 mg) was added tetrakis(triphenylphosphine)-palladium (37 mg). The mixture was degassed with N2 and heated in a microwave oven for 60 min at 120° C. The reaction mixture was concentrated under vacuum and purified by separation method K. K2CO3 was added to the reaction crude (in MeOH) and the mixture was stirred 4 h at it. The title compound was isolated by a separation method G. (Yield 6.2 mg).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09249127B2uspto-grants-2016_02