تفاعل #7593

ord-aeca40a5c11b49e09fe5ba429ff41801

المذيبات

ظروف التفاعل

درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصAfter extraction with ethyl acetate
  2. 2
    غسيلthe organic layer was washed with water
  3. 3
    تجفيفbrine, dried (MgSO4)
  4. 4
    أخرىthe solvent evaporated
  5. 5
    ترشيحThe solid was filtered off
  6. 6
    غسيلwashed with hexane
  7. 7
    أخرىdried under vacuum

الإجراء التجريبي

The starting material 5-benzyloxy-2-fluoro-4-methylnitrobenzene was obtained by adding benzyl bromide (3 ml, 25 mmol) to a solution of 2-fluoro-5-hydroxy-4-methylnitrobenzene (3.92 mg, 23 mmol) in DMF (70 ml) containing potassium carbonate (9.5 g, 68 mmol). After stirring for 3 hours at 60° C. the mixture was diluted with water and adjusted to pH2. After extraction with ethyl acetate, the organic layer was washed with water and then brine, dried (MgSO4) and the solvent evaporated. The solid was filtered off, washed with hexane and dried under vacuum to give 5-benzyloxy-2-fluoro-4-methylnitrobenzene (4.83 g, 80%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07087602B2uspto-grants-2006_08