反応 #90556

ord-52254e9e48e4418b87446d687f3fac69

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄washed with water (3×25 mL)
  2. 2
    乾燥The organic layer was dried over sodium sulphate
  3. 3
    濃縮concentrated
  4. 4
    その他to get the crude, which
  5. 5
    その他was purified through flash chromatography
  6. 6
    洗浄The compound 242 was eluted at 30% ethyl acetate in hexane

実験手順

To a solution of 13 (0.1 g, 0.404 mmol) in MeOH/H2O (1:1) was added nicotinaldehyde 241 (0.052 g, 0.484 mmol) and NaOH (0.032 g, 0.808 mmol). The reaction was stirred at RT for 6 h, diluted with chloroform and washed with water (3×25 mL). The organic layer was dried over sodium sulphate and concentrated to get the crude, which was purified through flash chromatography by using 100-200 mesh silica gel. The compound 242 was eluted at 30% ethyl acetate in hexane to afford yellow coloured solid (E)-6-methoxy-5-morpholino-2-(pyridin-3-ylmethylene)-2,3-dihydro-1H-inden-1-one 242.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09446047B2uspto-grants-2016_09