反応 #11347

ord-65102f31262e4021b5784cb373f3c5c1

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the reaction mixture was heated
  2. 2
    温度at reflux
  3. 3
    その他to yield a clear solution
  4. 4
    温度at reflux
  5. 5
    その他the solvent was removed in vacuo and excess HCl and thionyl chloride
  6. 6
    その他was chased by evaporation with dichloroethane

実験手順

Thionyl chloride (4 mL) was added to a suspension of the benzothiazole-6-sulfonic acid (0.60 g, 2.79 mmol) in dichloroethane (15 mL) and the reaction mixture was heated at reflux and dimethylformamide (5 mL) was added to the reaction mixture to yield a clear solution. After 1.5 hr. at reflux, the solvent was removed in vacuo and excess HCl and thionyl chloride was chased by evaporation with dichloroethane.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07098202B2uspto-grants-2006_08