反応 #671111

ord-0bd2e49c02b64619a54de44bd9042992

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度heated at 75° C. for 40 minutes
  2. 2
    温度cooled
  3. 3
    workup.ADDITIONpoured onto ice
  4. 4
    その他to provide a solid
  5. 5
    ろ過The solid was collected by suction filtration
  6. 6
    洗浄washed with water
  7. 7
    その他dried

実験手順

A solution of chlorosulfonic acid at 0° C. (5 mL, 75 mmol) was treated portionwise with 1-methylindoline (CAS No. [824-21-5], 1.96 g, 14.7 mmol), warmed to room temperature, heated at 75° C. for 40 minutes, cooled, and poured onto ice to provide a solid. The solid was collected by suction filtration, washed with water, and dried to provide 927 mg of the desired product.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06924304B2uspto-grants-2005_08