Diethyl (ethoxymethylene)malonate → HCID 10015075、化合物
反応式
[NH2:1][N:2]1[CH:6]=[CH:5][CH:4]=[CH:3]1.C(O[CH:10]=[C:11]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:12]([O:14][CH2:15][CH3:16])=[O:13])C>>[N:2]1([NH:1][CH:10]=[C:11]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH:6]=[CH:5][CH:4]=[CH:3]1参加物
3
反応条件
- 温度
- 125 °C
実験手順
A mixture of N-aminopyrrole (6.2 g, 75.5 mmol) and diethyl ethoxymethylenemalonate (18.2 mL, 90.6 mmol) was heated at 125° C. for 2 hours to give diethyl 2-((1H-pyrrol-1-ylamino)methylene)malonate as an intermediate and then diphenyl ether (22 mL) was added thereto. The resulting reaction mixture was heated under nitrogen atmosphere at 220° C. for 2 hours and ethanol produced during the reaction was removed by distillation. The reaction mixture with ethanol removed was cooled to room temperature and purified by silica gel chromatography. The target compound was yielded as a yellow solid (11.0 g, 53.3 mmol, 71% yield).
出典と根拠
- ORDレコード
- ord-a391657bc8a641878dde1cb5e6b92e04
- 出典データセット
- uspto-grants-2015_02
- 特許番号
- US08957102B2
反応ノート
読み込み中…