تفاعل #215851

ord-82bddaaa76b1434a962a544ffbe9ebaa

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىprepared
  2. 2
    درجة الحرارةThe resulting yellow solution was refluxed under a N2 atmosphere for 16 hours
  3. 3
    استخلاصThe reaction mixture was extracted with sodium hydroxide (1M, 2×200 mL)
  4. 4
    استخلاصextracted with ethyl acetate (3×200 mL)
  5. 5
    تجفيفdried (Na2SO4)
  6. 6
    أخرىevaporated

الإجراء التجريبي

To a solution of 8-chlorodibenz[b,f][1,4]oxazepine-10(11H)-carboxylic acid, hydrazide (1) (1.5 g, 5 mmol), prepared as described above in Example 1, and methyl 4-(4-pyridyl)butanoate (48) (2.4 g, 13 mmol), prepared as described above in Example 48, in toluene (250 mL) was added dimethylaluminumchloride (20.0 mmol). The resulting yellow solution was refluxed under a N2 atmosphere for 16 hours. The reaction mixture was allowed to cool to room temperature, followed by the addition of methanol (7 mL). The reaction mixture was extracted with sodium hydroxide (1M, 2×200 mL), and the aqueous extracts were combined and extracted with ethyl acetate (3×200 mL). The organic solutions were combined, dried (Na2SO4) and evaporated to yield 1.8 g of crude product as a thick oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05464830uspto-grants-1995_11