Methylamine → 2-Methyl-2,7-diazaspiro[4.4]nonane-1,3,8-trione
反応式
C([O:3][C:4](=O)[CH2:5][C:6]1([C:12]([O:14]CC)=O)[CH2:10][C:9](=[O:11])[NH:8][CH2:7]1)C.[CH3:18][NH2:19]>>[CH3:18][N:19]1[C:4](=[O:3])[CH2:5][C:6]2([CH2:10][C:9](=[O:11])[NH:8][CH2:7]2)[C:12]1=[O:14]参加物
3
反応条件
- 温度
- 220 °C
実験手順
A solution of 20.3 g (0.084 mole) 3-ethoxycarbonyl-5-oxo-3-pyrrolidineacetic acid ethyl ester [J. Org. Chem. 46, 2757 (1981)]in 40 ml of 40% aqueous methylamine was stirred at room temperature overnight, then placed in an oil bath and gradually heated to 220° C. over 30 minutes allowing volatiles to distill from the open flask. The crude product was crystallized from ethanol to afford 12.56 g of the title compound, mp 201°-204° C. Analysis calculated for C8H10N2O3 : C, 52.74; H, 5.53; N, 15.38. Found: C, 52.87; H, 5.60; N, 15.25.
後処理
- customplaced in an oil bath
- distillationto distill from the open flask
- customThe crude product was crystallized from ethanol
出典と根拠
- ORDレコード
- ord-7ee64ba62ec14495a07be778c93f97f5
- 出典データセット
- uspto-grants-1987_01
- 特許番号
- US04638067
反応ノート
読み込み中…