반응 #331552

ord-7b97ea2bf04a4caa9d38307dd6d88965

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooling
  2. 2
    세척the reaction solution was washed with water
  3. 3
    건조a saturated aqueous sodium chloride solution, dried over magnesium sulfate
  4. 4
    농축the solvent was concentrated

실험 절차

To a solution of N-isopropyl-2,2-dimethyl-3-oxo-N-[(3R)-piperidin-3-yl]-4-[2-(propionylamino)ethyl]-7-(trifluoromethyl)-3,4-dihydro-2H-1,4-benzoxazine-6-carboxamide hydrochloride (3.0 g) in chloroform (25 ml) were added successively triethylamine (0.98 ml) and 1-chloroethyl chloroformate (0.63 ml) under ice-cooling, and the mixture was stirred at room temperature overnight. After the reaction was completed, the reaction solution was washed with water and a saturated aqueous sodium chloride solution, dried over magnesium sulfate, and the solvent was concentrated to give the title compound (3.55 g) as white amorphous. The obtained title compound was used in the next reaction without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08658639B2uspto-grants-2014_02