反応 #161012

ord-843994d8348c424f9d7abf57da5a86a0

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄The reaction solution was successively washed with water
  2. 2
    乾燥a 10% aqueous potassium hydrogensulfate solution, a saturated aqueous sodium hydrogencarbonate solution and saturated brine, and it was dried with anhydrous sodium sulfate
  3. 3
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure
  4. 4
    洗浄the obtained crystal was washed with diethyl ether

実験手順

1.38 g (9.3 mmol) of 2-oxo-1-imidazolidinecarbonyl chloride was added to a solution of 2.17 g (9.3 mmol) of 1-aminocyclohexanecarboxylic acid phenylmethyl ester and 1.04 g (10 mmol) of triethylamine in 100 ml of chloroform, and the mixture was stirred at 60° C. for 4 days. The reaction solution was successively washed with water, a 10% aqueous potassium hydrogensulfate solution, a saturated aqueous sodium hydrogencarbonate solution and saturated brine, and it was dried with anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the obtained crystal was washed with diethyl ether to obtain 2.64 g (82%) of the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08829209B2uspto-grants-2014_09