反応 #60948

ord-99e1bb6a5152417c91d818557afbaf55

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他After evaporation of the volatiles 15 ml 5N HCl
  2. 2
    workup.ADDITIONwas added
  3. 3
    抽出the mixture was extracted 3× with ethylacetate
  4. 4
    その他The solvent was removed under vacuum

実験手順

A mixture of 1 g (4 mmol) 2-Chloro-5-sulfino-benzoic acid and 0.62 g (20 mmol) Methylamine in 10 ml dioxane was stirred for 3 h at room temperature. After evaporation of the volatiles 15 ml 5N HCl was added and the mixture was extracted 3× with ethylacetate. The solvent was removed under vacuum to yield 0.724 g (72%) of the title compound as amorphous white solid. MS (m/e): 248.1 (MH−, 100%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07427612B2uspto-grants-2008_09