반응 #9669

ord-af7ba1a7ab60417d86d4e7b9a1184323

반응 방정식

O=S(=O)(Cl)Cl
Sulfuryl chloride
Fc1ccc2sc(S)nc2c1
5-fluoro-1,3-benzothiazole-2-thiol
Fc1ccc2sc(Cl)nc2c1
2-Chloro-5-fluoro-1,3-benzothiazole

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated at 60° C. for 30 minutes
  2. 2
    온도The resulting solution was cooled to rt
  3. 3
    workup.ADDITIONpoured onto ice
  4. 4
    여과The title compound was collected by filtration
  5. 5
    세척washed with water
  6. 6
    기타dried under vacuum
  7. 7
    기타The solid obtained
  8. 8
    기타was used without further purification

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091228B2uspto-grants-2006_08