تفاعل #85919

ord-ecdf40fd281e46aeb409fcdd9637bab6

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىreacted at 100° C. for 3 hours
  2. 2
    استخلاصextracted by EA
  3. 3
    غسيلwashed by 2M NaOH
  4. 4
    تجفيفdried over Na2SO4
  5. 5
    تركيزconcentrated
  6. 6
    أخرىpurified by flash chromatography

الإجراء التجريبي

1-(4-aminophenyl)piperidin-4-ol (600 mg, 3.12 mmol), HBr (14 mL, 48%), was mixed and cooled to 0° C., the solution of NaNO2 (215 mg, 3.12 mmol) in 2.3 mL water was added in. the mixture was stirred for 15 minutes, the solution of CuBr (246 mg, 1.72 mmol) in HBr (4.4 mL 4.8%) was added and reacted at 100° C. for 3 hours. 2M NaOH solution was added, extracted by EA, washed by 2M NaOH, dried over Na2SO4, concentrated and purified by flash chromatography. (PE:EA=3:1) to give 520 mg pale brown solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09434726B2uspto-grants-2016_09