反応 #47196

ord-f46bacf9bd4f4633ae87241f3c9c8450

反応条件

温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The vial was capped
  2. 2
    温度The reaction was cooled down to room temperature
  3. 3
    その他quenched by drop wise addition of methanol (2 mL)
  4. 4
    workup.STIRRINGstirred at room temperature for 30 minutes
  5. 5
    ろ過filtered
  6. 6
    workup.STIRRINGstirred with Dowex 50WX2-200 resin (1 g) for 26.5 hours
  7. 7
    ろ過The resin was filtered
  8. 8
    洗浄washed with methanol (20 mL) and 10% aqueous ammonia (50 mL)
  9. 9
    その他The solvent was removed under vacuum
  10. 10
    その他The material was used without any further purification in the next step

実験手順

To a vial containing 4-aminonaphthalene-1-carbonitrile (0.59 mmol) was added BH3.THF (1M solution (1.2 mmol). The vial was capped and stirred at 70° C. for 19.5 hours. The reaction was cooled down to room temperature and quenched by drop wise addition of methanol (2 mL), stirred at room temperature for 30 minutes, filtered and stirred with Dowex 50WX2-200 resin (1 g) for 26.5 hours. The resin was filtered, washed with methanol (20 mL) and 10% aqueous ammonia (50 mL). The solvent was removed under vacuum. The material was used without any further purification in the next step.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07741479B2uspto-grants-2010_06