Reaktion #542797

ord-044f9a7142ce4d6db3e180766276c496

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction mixture was quenched with aqueous, saturated sodium carbonate solution
  2. 2
    workup.STIRRINGstirred for 10 minutes
  3. 3
    SonstigeThe organic layer was separated
  4. 4
    Einengenconcentrated under reduced pressure

Vorschrift

1-Chloro-N,N,2-trimethylprop-1-en-1-amine (2.012 ml, 15.05 mmol) was added to a solution of N-((7-bromo-4-fluoro-9-(2-hydroxyethyl)-2-methoxy-9H-xanthen-9-yl)carbamothioyl)-benzamide (8 g, 15.05 mmol) in DCM (3 ml). The reaction mixture was stirred at RT for 8 hours. The reaction mixture was quenched with aqueous, saturated sodium carbonate solution and stirred for 10 minutes. The organic layer was separated and concentrated under reduced pressure to afford crude N-(7′-bromo-4′-fluoro-2′-methoxy-5,6-dihydrospiro[[1,3]thiazine-4,9′-xanthen]-2-yl)benzamide (7.7 g, 15.00 mmol, 100% yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08497264B2uspto-grants-2013_07