1,3-Diethyl 2-oxopropanedioate → Diethyl 2-(2-methyl-2-propionylhydrazono)malonate
反応式
[CH3:1][N:2]([C:4](=[O:7])[CH2:5][CH3:6])[NH2:3].O=[C:9]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[C:10]([O:12][CH2:13][CH3:14])=[O:11]>C1(C)C=CC=CC=1>[CH3:1][N:2]([C:4](=[O:7])[CH2:5][CH3:6])[N:3]=[C:9]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[C:15]([O:17][CH2:18][CH3:19])=[O:16]参加物
4
実験手順
A solution of N-methylpropionohydrazide (18.78 g, 183.9 mmol) and diethyl ketomalonate (56.1 mL, 368 mmol) in toluene (136 mL) was refluxed with a Dean-Stark trap for 4 hours. The reaction mixture was concentrated under reduced pressure to give the crude material that was purified by silica gel flash column chromatography (100% hexanes to 5 to 10% EtOAc in hexanes) to afford 23 g (49%) of the desired product.
後処理
- concentrationThe reaction mixture was concentrated under reduced pressure
- customto give the crude material that
- customwas purified by silica gel flash column chromatography (100% hexanes to 5 to 10% EtOAc in hexanes)
出典と根拠
- ORDレコード
- ord-5cdca83ee7f64971b5c07200968b6b9d
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07732616B2
反応ノート
読み込み中…