تفاعل #8006

ord-e9eae8e4020a414d90a4fd0e994de72c

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe mixture was heated
  2. 2
    workup.STIRRINGthe mixture was stirred further at the same temperature for 4 hours
  3. 3
    درجة الحرارةcooled
  4. 4
    ترشيحThe precipitate was collected by filtration
  5. 5
    غسيلthoroughly washed with water
  6. 6
    أخرىdried

الإجراء التجريبي

To a solution of ethyl 2-ethoxycarbonyl-4-(3-fluoro-4-methylphenyl)-2-hydroxy-4-oxobutanoate (8.41 9, 25.8 mmol) in isopropanol (100 mL) was added hydrazine monohydrate (2.84 g, 56.8 mmol), and the mixture was heated under stirring at 100 for 6 hours. Then, 2 mol/L sodium hydroxide was added, and the mixture was stirred further at the same temperature for 4 hours. The reaction mixture was ice-cooled, and concentrated hydrochloric acid was added to acidify the system. The precipitate was collected by filtration, thoroughly washed with water and dried to yield the title compound as a slightly yellow crystalline powder (5.67 g, 87.7%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07087606B2uspto-grants-2006_08