HCID 15677249、化合物 → HCID 178440053、化合物
反応式
[N:1](=[C:3]([C:7](=[O:9])[CH3:8])[C:4](=O)[CH3:5])O.C[NH:11][CH:12](C(O)=O)[CH2:13][CH2:14][CH3:15]>C(#N)C>[C:7]([C:3]1[NH:1][C:12]([CH2:13][CH2:14][CH3:15])=[N:11][C:4]=1[CH3:5])(=[O:9])[CH3:8]参加物
4
実験手順
To 40 g (0.31 moles) of 3-oximino-2,4-pentanedione dissolved in 297 ml of acetonitrile was added 40.64 g (0.31 moles) of methyl d,l-norvaline. The reaction mixture was refluxed 21.2 h under nitrogen, cooled, then concentrated in vacuo. The resulting oil was dissolved in 50 ml of ethanol and 140 ml of 10% aqueous sodium hydroxide. After 4 h of reflux, the cooled mixture was extracted with ethyl acetate (900 ml total) and dried over anhydrous sodium sulfate. Removal of the solvent in vacuo afforded 0.16 moles (51% yield) of 5-acetyl-4-methyl-2-propylimidazole.
後処理
- temperatureThe reaction mixture was refluxed 21.2 h under nitrogen
- temperaturecooled
- concentrationconcentrated in vacuo
- dissolutionThe resulting oil was dissolved in 50 ml of ethanol
- temperatureAfter 4 h of reflux
- extractionthe cooled mixture was extracted with ethyl acetate (900 ml total)
- dry with materialdried over anhydrous sodium sulfate
- customRemoval of the solvent in vacuo
出典と根拠
- ORDレコード
- ord-1437becb9354433bb7b3bb95f009b63b
- 出典データセット
- uspto-grants-1983_07
- 特許番号
- US04395547
反応ノート
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