تفاعل #45936

ord-1a59dbac1df94d85990d11a3d8f7174d

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter cooling to rt
  2. 2
    استخلاصextracted with EtOAc (2×15 mL)
  3. 3
    غسيلThe combined organic layers were washed with brine
  4. 4
    تجفيفdried over sodium sulfate
  5. 5
    أخرىEvaporation of the solvent in vacuuo

الإجراء التجريبي

To a stirred solution of 3-nitrophenol (2 mmol) in DMF (6 mL) at rt, solid potassium carbonate (4 mmol) was added. A solution of the mesylate of N,N-diethylaminopropanol (2.2 mmol) in DMF (2 mL) was then added to the reaction mixture and heated to 80° C. until completion, according to General Procedure Q1, as indicated by TLC or HPLC. After cooling to rt, the reaction mixture was then treated with cold H2O (15 mL), and extracted with EtOAc (2×15 mL). The combined organic layers were washed with brine and dried over sodium sulfate. Evaporation of the solvent in vacuuo afforded the desired N,N-diethyl-N-[3-(3-nitrophenoxy)propyl]amine. The crude product was used directly for further transformation.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07737285B2uspto-grants-2010_06