反応 #57558

ord-c7aee23be9fa4d6ea3058bed23397285

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄The dichloromethane was washed with water and brine
  2. 2
    乾燥dried over Na2SO4
  3. 3
    ろ過filtered
  4. 4
    濃縮concentrated in vacuo

実験手順

To 0.838 g of L-valine methyl ester hydrochloride in 15 mL of dichloromethane, cooled in an ice bath, 1.34 g of 4-bromobenzenesulfonyl chloride was added followed by 2.79 mL of triethylamine. The mixture was stirred at room temperature overnight and then diluted with dichloromethane. The dichloromethane was washed with water and brine, dried over Na2SO4, filtered, and concentrated in vacuo to provide 1.77 g of methyl N-[(4-bromophenyl)sulfonyl]-L-valinate as a colorless solid. Yield ˜100%. m.p. 88-90° C.; MS: 348.2 (M−H)−.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07420001B2uspto-grants-2008_09