تفاعل #47196

ord-f46bacf9bd4f4633ae87241f3c9c8450

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
70°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07741479B2uspto-grants-2010_06