Methylamine → 2-Methyl-2,7-diazaspiro[4.4]nonane-1,3,8-trione
反応式
C([O:3][C:4]([C:6]1([CH2:12][C:13]([O:15]CC)=O)[CH2:10][C:9](=[O:11])[NH:8][CH2:7]1)=O)C.[CH3:18][NH2:19]>>[CH3:18][N:19]1[C:13](=[O:15])[CH2:12][C:6]2([CH2:10][C:9](=[O:11])[NH:8][CH2:7]2)[C:4]1=[O:3]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 12.6 g of 2-methyl-2,7-diazaspiro[4.4]nonane-1,3,8-trione, mp 201-204° C.
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-6ba53aa765d24a9d9c301101944c2363
- 出典データセット
- uspto-grants-1992_03
- 特許番号
- US05097032
反応ノート
読み込み中…