반응 #47196

ord-f46bacf9bd4f4633ae87241f3c9c8450

반응 조건

온도
70°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07741479B2uspto-grants-2010_06