反応 #46116

ord-cc7cdf4d90fc4c72980716ddfe9808c6

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONabove is introduced into a hermetically closed vessel
  2. 2
    workup.ADDITIONcontaining
  3. 3
    その他After this time period, the solvent and the reagent are removed
  4. 4
    濃縮by concentrating under reduced pressure
  5. 5
    ろ過is collected by filtration
  6. 6
    洗浄washed with methanol
  7. 7
    その他dried

実験手順

2-Chloro-5-nitrobenzenesulphonamide (5 g) prepared in the Step above is introduced into a hermetically closed vessel containing a mixture of dioxane (70 mL) and cyclopropylamine (3.5 mL). The hermetically closed vessel is placed in an oven at 100° C. for 24 hours. After this time period, the solvent and the reagent are removed by concentrating under reduced pressure. The residue is taken up in methanol (20 mL) and the insoluble material, which contains the title product, is collected by filtration, washed with methanol and dried.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07741320B2uspto-grants-2010_06