반응 #215851
ord-82bddaaa76b1434a962a544ffbe9ebaa
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후처리
- 1기타prepared
- 2온도The resulting yellow solution was refluxed under a N2 atmosphere for 16 hours
- 3추출The reaction mixture was extracted with sodium hydroxide (1M, 2×200 mL)
- 4추출extracted with ethyl acetate (3×200 mL)
- 5건조dried (Na2SO4)
- 6기타evaporated
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.