반응 #215851

ord-82bddaaa76b1434a962a544ffbe9ebaa

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타prepared
  2. 2
    온도The resulting yellow solution was refluxed under a N2 atmosphere for 16 hours
  3. 3
    추출The reaction mixture was extracted with sodium hydroxide (1M, 2×200 mL)
  4. 4
    추출extracted with ethyl acetate (3×200 mL)
  5. 5
    건조dried (Na2SO4)
  6. 6
    기타evaporated

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05464830uspto-grants-1995_11