反応式
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]2[O:6][C:7]3[CH:18]=[CH:17][CH:16]=[CH:15][C:8]=3[CH2:9][N:10]([C:11]([NH:13][NH2:14])=[O:12])[C:4]=2[CH:3]=1.[N:21]1[CH:26]=[CH:25][C:24]([CH2:27][CH2:28][CH2:29][C:30](OC)=[O:31])=[CH:23][CH:22]=1.[Cl-].C[Al+]C.CO>C1(C)C=CC=CC=1>[O:31]=[C:30]([NH:14][NH:13][C:11]([N:10]1[CH2:9][C:8]2[CH:15]=[CH:16][CH:17]=[CH:18][C:7]=2[O:6][C:5]2[CH:19]=[CH:20][C:2]([Cl:1])=[CH:3][C:4]1=2)=[O:12])[CH2:29][CH2:28][CH2:27][C:24]1[CH:23]=[CH:22][N:21]=[CH:26][CH:25]=1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
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.
後処理
- customprepared
- temperatureThe resulting yellow solution was refluxed under a N2 atmosphere for 16 hours
- extractionThe reaction mixture was extracted with sodium hydroxide (1M, 2×200 mL)
- extractionextracted with ethyl acetate (3×200 mL)
- dry with materialdried (Na2SO4)
- customevaporated
出典と根拠
- ORDレコード
- ord-89ece8e93a4f4b2eafe3c7c96c3a21d9
- 出典データセット
- uspto-grants-1996_11
- 特許番号
- US05576315
関連ノート
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