Reaktion #58559

ord-2996ca1e74824e76982146f3153ba8e9

Lösungsmittel

Reaktionsbedingungen

Temperatur
22°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationNext, the reaction mixture was filtered
  2. 2
    Einengenconcentrated
  3. 3
    workup.DISSOLUTIONthe residue was dissolved in anhydrous MeOH (25 ml)
  4. 4
    EinengenThe MeOH was concentrated
  5. 5
    Sonstigetriturated with ether

Vorschrift

The product of step f) (1.16 g, 4.3 mmol) in dichloroethane (21 ml) was treated with K2CO3 (2.38 g, 17.2 mmol) and Ace-Cl (1.86 ml, 17.2 mmol) at 800C for 16 hours. Next, the reaction mixture was filtered, concentrated and the residue was dissolved in anhydrous MeOH (25 ml) and stirred for 1 hour at 22° C. The MeOH was concentrated and triturated with ether to give 874 mg (94%) of the subtitle compound. MS calculated for C10H13NS+H 180, observed 180.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07423056B2uspto-grants-2008_09