تفاعل #316215

ord-86778dcdb2d24ed99375f8c4bd7c3611

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe suspension was hermetically sealed and, in this state
  2. 2
    استخلاصthe mixture was extracted
  3. 3
    غسيلThe dichloromethane layer was washed with water and saturated brine
  4. 4
    تجفيفwas dried over magnesium sulfate
  5. 5
    أخرىThe solvent was removed by distillation under the reduced pressure
  6. 6
    أخرىthe residue was purified by column chromatography

الإجراء التجريبي

2-Amino-pyridine-3-carbaldehyde (100 mg) and 2-chloro-1-phenyl-ethanone (127 mg) were suspended in a 5 N aqueous sodium hydroxide solution (0.6 ml), and the suspension was hermetically sealed and, in this state, was allowed to stand for 3 days. The reaction solution was neutralized with 10% hydrochloric acid. Dichloromethane was then added thereto, and the mixture was extracted. The dichloromethane layer was washed with water and saturated brine and was dried over magnesium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by column chromatography using chloroform-methanol to give 2-phenyl-[1,8]naphthyridin-3-ol (23 mg, yield 13%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07560558B2uspto-grants-2009_07