Methanol → Ethyl 2,5-dioxopyrrole-1-carboxylate
反応式
Cl[C:2]([O:4][CH2:5][CH3:6])=[O:3].[C:7]1(=[O:13])[NH:11][C:10](=[O:12])[CH:9]=[CH:8]1.C(N(CC)CC)C.CO>CN(C)C=O.C(Cl)(Cl)Cl.CCCCCC>[CH2:5]([O:4][C:2]([N:11]1[C:7](=[O:13])[CH:8]=[CH:9][C:10]1=[O:12])=[O:3])[CH3:6]参加物
8
実験手順
Ethyl chloroformate (0.38 ml, 4 mmol) was added dropwise to a stirred solution maleimide (0.3 g, 3 mmol) and triethylamine (0.5 ml, 3.5 mmol) in dimethylformamide (2 ml) at 0-5° C. The reaction mixture was allowed to warm to room temperature and stand for 4 h. Methyl alcohol (1 ml) was added, diluted with chloroform (20 ml) and washed with water (3×10 ml). The chloroform solution was dried (Na2SO4) and concentrated in vacuum. The residue was purified in chloroform and hexane on a silica gel column to give N-ethoxycarbonyl-maleimide (yield 41%).
後処理
- washwashed with water (3×10 ml)
- dry with materialThe chloroform solution was dried (Na2SO4)
- concentrationconcentrated in vacuum
- customThe residue was purified in chloroform
出典と根拠
- ORDレコード
- ord-3ae2f3dd4c58410ab647411160b89d2a
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09273304B2
反応ノート
読み込み中…
