Hydrochloric Acid → HCID 12674909、化合物
反応式
[C:1]([O:6][CH3:7])(=[O:5])/[CH:2]=[CH:3]/[CH3:4].[N+:8]([CH2:11][CH2:12][CH3:13])([O-:10])=[O:9].Cl>C(#N)C.O>[CH3:4][CH:3]([CH:11]([N+:8]([O-:10])=[O:9])[CH2:12][CH3:13])[CH2:2][C:1]([O:6][CH3:7])=[O:5]参加物
6
実験手順
A solution of 4 g (40 mmol) of methyl crotonate and 4.72 g (53 mmol) of 1-nitropropane in 20 mL of acetonitrile was treated with 6 mL (40 mmol) of 1,8-diazobicyclo[5.4.0]undec-7-ene (DBU). After stirring for 22 h at room temperature the reaction mixture was diluted with water and acidified with 2N HCl. The solution was extracted with Et2O and the Et2O layer was washed with brine, dried and concentrated. The residue was chromagraphed on a flash column using 10% Et2O-Hexane to isolate 6.41 g (85%) of the title compound.
後処理
- extractionThe solution was extracted with Et2O
- washthe Et2O layer was washed with brine
- customdried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-792a5b228d6f4814a5f607fdfb0b8d3c
- 出典データセット
- uspto-grants-1997_05
- 特許番号
- US05629322
反応ノート
読み込み中…