反応 #11721

ord-03d958e6728f4420bdfbc1d54303f87c

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to warm to ambient temperature
  2. 2
    洗浄washed with 10% citric acid
  3. 3
    その他The organic layer was separated
  4. 4
    乾燥dried over magnesium sulfate
  5. 5
    ろ過filtered
  6. 6
    濃縮concentrated in vacuo

実験手順

To a solution of (3R)-1-(4-fluoro-benzyl)-3-methyl-piperazine (3 g, 14.4 mmol) in dichloromethane (40 mL) was added triethylamine (2.0 mL, 14.4 mmol). The reaction was cooled to 0° C. and chloroacetyl chloride was added (1.1 mL, 14.4 mmol). The reaction was allowed to warm to ambient temperature and stirred for 2 hours. The reaction is diluted with dichloromethane and washed with 10% citric acid. The organic layer was separated, dried over magnesium sulfate, filtered and concentrated in vacuo. Chromatography on silica gel gave the title compound (3.9 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07098212B2uspto-grants-2006_08