反応 #84514

ord-ba1c5d5cbe08443c89b0f722fa30537f

反応条件

温度
150°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture was cooled to rt
  2. 2
    濃縮concentrated in vacuo
  3. 3
    その他The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=1:1)

実験手順

A mixture of (Z)-3-amino-N-(3-trifluoromethyl-4-morpholinophenyl)but-2-enamide (4.0 g, 12.1 mmol) and triethyl orthoacetate (10 mL) was stirred at 150° C. overnight. The mixture was cooled to rt and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=1:1) to give the title compound as a pale yellow solid (3.00 g, 70%). The compound was characterized by the following spectroscopic data:

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09434695B2uspto-grants-2016_09