Reaktion #9231

ord-740e84ce00124f83a802a02af18c14b6

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe result precipitate was filtered off
  2. 2
    Waschenwashed with water and MeOH
  3. 3
    Sonstigedried under vacuum

Vorschrift

A suspension of 2-amino-6-(4′-fluorophenoxy)-benzothiazole (associated with 2.0 eq of KBr salt, 2.50 g, 5.02 mmol) in 10 mL pyridine was treated dropwise with methyl chlorothioformate (0.65 mL, 7.53 mmol, 01.5 eq). It was stirred at room temperature for about 1 hour, and was poured into 40 mL ice water. The mixture was acidified slowly with 1 M HCl solution. The result precipitate was filtered off, washed with water and MeOH, and dried under vacuum to give 1.18 g (65%) desired compound. LC/MS 334.9 (M+1); LC retention time 3.70 min.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07091227B2uspto-grants-2006_08