Methyl morpholine oxide → 8-Formyl-2-methyl-4-oxo-4H-1-benzopyran-5-carbonitrile
反応式
Br[CH:2](Br)[C:3]1[C:12]2[O:11][C:10]([CH3:13])=[CH:9][C:8](=[O:14])[C:7]=2[C:6]([C:15]#[N:16])=[CH:5][CH:4]=1.C[N+]1([O-])CC[O:22]CC1>C(#N)C>[CH:2]([C:3]1[C:12]2[O:11][C:10]([CH3:13])=[CH:9][C:8](=[O:14])[C:7]=2[C:6]([C:15]#[N:16])=[CH:5][CH:4]=1)=[O:22]参加物
4
実験手順
260 mg (0.72 mmol) of 8-(dibromomethyl)-2-methyl-4-oxo-4H-chromene-5-carbonitrile are heated with 187 mg (1.6 mmol) of N-methylmorpholine N-oxide with the addition of molecular sieves in 15 ml of acetonitrile under reflux overnight. After filtration through kieselguhr, the solvent is removed in vacuo, and the residue is purified by preparative HPLC. 23 mg (15% of theory) of the title compound are obtained.
後処理
- temperatureunder reflux overnight
- filtrationAfter filtration through kieselguhr
- customthe solvent is removed in vacuo
- customthe residue is purified by preparative HPLC
出典と根拠
- ORDレコード
- ord-ddce7f24a8f542deb19af123e9a9deb8
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08058447B2
反応ノート
読み込み中…