反応 #556341

ord-10cb1f4f0d3c4988ba3d4031e0193416

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他reaction mixture at room temperature for 14 hours
  2. 2
    抽出by extracting the resultant
  3. 3
    その他reaction mixture with ethyl acetate (50 mL) three times
  4. 4
    洗浄the organic phase was washed sequentially with water (50 mL)
  5. 5
    乾燥a saturated saline (50 mL) and was dried over anhydrous sodium sulfate
  6. 6
    workup.DISTILLATIONFrom the organic phase, the solvent was distilled off under reduced pressure

実験手順

5-bromo-2,3-dihydro-1H-inden-1-one (2.0 g) was dissolved in methanol (20 mL), and to the resultant solution, sodium borohydride (0.54 g) was added at room temperature, followed by stirring the resultant reaction mixture at room temperature for 14 hours. To the reaction mixture, 1M hydrochloric acid (50 mL) was added, followed by extracting the resultant reaction mixture with ethyl acetate (50 mL) three times, and the organic phase was washed sequentially with water (50 mL) and a saturated saline (50 mL) and was dried over anhydrous sodium sulfate. From the organic phase, the solvent was distilled off under reduced pressure to obtain the subject compound (2.0 g) as a pale yellow solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08629102B2uspto-grants-2014_01