Реакция #9669

ord-af7ba1a7ab60417d86d4e7b9a1184323

Реагенты

Нет

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураheated at 60° C. for 30 minutes
  2. 2
    ТемператураThe resulting solution was cooled to rt
  3. 3
    workup.ADDITIONpoured onto ice
  4. 4
    ФильтрацияThe title compound was collected by filtration
  5. 5
    Промывкаwashed with water
  6. 6
    Другоеdried under vacuum
  7. 7
    ДругоеThe solid obtained
  8. 8
    Другоеwas used without further purification

Методика

Sulfuryl chloride (50 μL, 0.65 mmol) was added neat to 5-fluoro-1,3-benzothiazole-2-thiol (100 mg, 0.54 mmol). The mixture was stirred at ambient temperature for 1 h, then heated at 60° C. for 30 minutes. The resulting solution was cooled to rt, and poured onto ice. The title compound was collected by filtration, washed with water, and dried under vacuum. The solid obtained was used without further purification; LC-MS m/z 188.1 (MH+), ret. time 3.27 min.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07091228B2uspto-grants-2006_08