反応 #69030

ord-50b89bd3495147078f6a4cd843f35adc

溶媒

反応条件

温度
90°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction mixture was cooled to room temperature
  2. 2
    ろ過The resulting colorless precipitate was filtered
  3. 3
    洗浄washed with water
  4. 4
    その他dried in vacuo

実験手順

A mixture of 5-bromo-1,2,3-trifluorobenzene (2.5 g, 11.8 mmol), morpholine (1.0 mL, 11.8 mmol), K2CO3 (1.6 g, 11.8 mmol) and DMSO (2 mL) in a sealed tube was heated up to 90° C. for 2.5 h. The reaction mixture was cooled to room temperature and diluted with water. The resulting colorless precipitate was filtered, washed with water, and dried in vacuo to afford 4-(5-bromo-2,3-difluorophenyl)morpholine in 76% yield. 1H NMR (CDCl3, 400 MHz) δ 6.91-6.87 (m, 1H), 6.75-6.72 (m, 1H), 3.80-3.78 (m, 4H), 3.04-3.02 (m, 4H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08530480B2uspto-grants-2013_09