反応 #72716

ord-4a9fdad254f04dc1b4dd32db485b3fe6

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooled again
  2. 2
    抽出Extraction of the aqueous solution
  3. 3
    乾燥Then, the combined organic layers were dried over MgSO4
  4. 4
    その他the solvent was removed by reduced pressure
  5. 5
    その他The residue was triturated
  6. 6
    ろ過the product was collected by filtration in 80% yield

実験手順

To a stirred solution of glycine (100 mmol) and NaOH (100 mmol) in water (300 ml), at 5° C., o-chloro-benzoyl chloride (110 mmol) was added in small portions. The reaction mixture was stirred for 30 minutes at room temperature, then cooled again and acidified to pH=2 by addition of 6 M HCl. Extraction of the aqueous solution was performed with EtOAc. Then, the combined organic layers were dried over MgSO4 and the solvent was removed by reduced pressure. The residue was triturated in boiling chloroform, and the product was collected by filtration in 80% yield.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541428B2uspto-grants-2013_09