反応 #69403

ord-23547f41ebaf4837bd1d7a5c574a0f8c

溶媒

反応条件

温度
170°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with EtOAc (50 ml×3)
  2. 2
    洗浄The combined organic phases were washed with a saturated solution of NaCl (30 ml×2)
  3. 3
    濃縮concentrated under reduced pressure
  4. 4
    その他The product was purified by column chromatography

実験手順

In a microwave vial were dissolved 2-bromo-1-phenylethanone (95 mg, 0.478 mmol) and 3,4-diethoxybenzamide (100 mg, 0.478 mmol) in DMF (5 ml) and the reaction was heated at 170° C. for 40 min. The reaction mixture was poured in a saturated solution of NaHCO3 and extracted with EtOAc (50 ml×3). The combined organic phases were washed with a saturated solution of NaCl (30 ml×2) and concentrated under reduced pressure. The product was purified by column chromatography using CH2Cl2:MeOH (95:5) to yield 25 mg (17%) of the product. MS (EI) m/z: 310 (M+)

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08530503B2uspto-grants-2013_09