反応 #46126

ord-096df4f75def4fc0af51d27068220afa

溶媒

反応条件

温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他obtained
  2. 2
    workup.DISSOLUTIONhas completely dissolved
  3. 3
    ろ過the suspension is discharged by filtration in the hot state
  4. 4
    workup.ADDITIONby adding 12N HCl
  5. 5
    その他The precipitate obtained
  6. 6
    ろ過is collected by filtration
  7. 7
    洗浄washed with water
  8. 8
    その他dried

実験手順

A suspension of 2-fluoro-5-methylbenzenesulphonamide (5.3 mmol), obtained according to the process described in Step A of Example 1 starting from 2-fluoro-5-methylaniline, in water (50 mL) is heated at 70° C. and then NaOH 10% w/v is added dropwise until the compound has completely dissolved. Potassium permanganate (3 g) is added in small portions. After stirring for 4 hours, the suspension is discharged by filtration in the hot state and the filtrate is brought to pH 1 by adding 12N HCl. The precipitate obtained is collected by filtration, washed with water and dried to yield the title product in the form of a white solid.

出典

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