反応式
[H-].[Na+].[CH3:3][C:4]1([CH3:17])[CH2:9][NH:8][C:7]2=[CH:10][C:11]3[C:12](=[N:14][O:15][N:16]=3)[CH:13]=[C:6]2[O:5]1.Cl.Cl[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][N+:21]=1[O-:26]>CN(C)P(N(C)C)(N(C)C)=O>[CH3:3][C:4]1([CH3:17])[CH2:9][N:8]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][N+:21]=2[O-:26])[C:7]2=[CH:10][C:11]3[C:12](=[N:14][O:15][N:16]=3)[CH:13]=[C:6]2[O:5]1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
To a suspension of 215 mg sodium hydride (60%) in 5 ml hexamethylphosphoramide, were added 500 mg 7,8-dihydro-6,6-dimethyl-6H-[1,2,5]oxadiazolo[3,4-g][1,4]benzoxazine and 486 mg 2-chloropyridine N-oxide hydrochloride in that order, and the mixture was stirred at room temperature for six hours. The reaction mixture was poured into ice water, the resulting mixture was extracted with ethyl acetate, the extract was washed with an aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and the solvents were distilled off from the dried solution. The residue was subjected to column chromatography on silica gel, and the crystals obtained by elution with a 2:1 mixture of chloroform and acetone were recrystallized from 6 ml ethanol, giving 409 mg of 2-(7,8-dihydro-6,6-dimethyl-6H-[1,2,5]oxadiazolo[3,4-g][1,4]benzoxazin-8-yl)pyridine 1-oxide.
後処理
- extractionthe resulting mixture was extracted with ethyl acetate
- washthe extract was washed with an aqueous solution of sodium chloride
- dry with materialdried over anhydrous magnesium sulfate
- distillationthe solvents were distilled off from the dried solution
- customthe crystals obtained by elution with a 2:1 mixture of chloroform and acetone
- customwere recrystallized from 6 ml ethanol
出典と根拠
- ORDレコード
- ord-6eb77da0f6344760833c67c4d7103f6b
- 出典データセット
- uspto-grants-1994_01
- 特許番号
- US05278158
関連ノート
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