تفاعل #2295970

ord-8b1840ddb1254fb5b94dbbad3d749db4

المذيبات

ظروف التفاعل

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

المعالجة

  1. 1
    ترشيحOn completion, the reaction mixture was filtered
  2. 2
    غسيلthrough celite washing with ethanol and ethylacetate
  3. 3
    استخلاصThe filtrate was extracted with ethyl acetate
  4. 4
    غسيلthe combined organic layers were washed with water
  5. 5
    أخرىdried
  6. 6
    تركيزconcentrated under reduced pressure

الإجراء التجريبي

To stirred solution of methyl 5-bromo-2-chloro-3-nitrobenzoate (3.4 g, 11.6 mmol) in ethanol (19 mL) was added ammonium chloride (3.4 g, 57.8 mmol) dissolved in water (30 mL) and iron powder (5.16 g, 92.5 mmol). The reaction mixture was heated at 80° C. for 1 h. On completion, the reaction mixture was filtered through celite washing with ethanol and ethylacetate. The filtrate was extracted with ethyl acetate and the combined organic layers were washed with water, dried and concentrated under reduced pressure to give methyl 3-amino-5-bromo-2-chlorobenzoate (2.8 g, 92.1%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09376422B2uspto-grants-2016_06