反応式
[CH2:1]([N:8]1[CH2:18][CH2:17][C:11]2([O:15][C:14](=[O:16])[NH:13][CH2:12]2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].[CH2:21](I)[CH3:22].Cl>O.CN(C)C=O>[CH2:21]([N:13]1[CH2:12][C:11]2([CH2:17][CH2:18][N:8]([CH2:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[CH2:9][CH2:10]2)[O:15][C:14]1=[O:16])[CH3:22]参加物
7
実験手順
A mixture of 16.5 g 8-benzyl-1-oxa-3,8-diazaspiro[4.5]decan-2-one, 6.6 g, 50% suspension of sodium hydride in mineral oil, 15 g ethyl iodide and 70 ml N,N-dimethylformamide is heated at 90° for one hour. The mixture is poured into 150 ml water and the resulting mixture acidified with 10 N hydrochloric acid. The mixture is extracted with two 100 ml portions of hexane. The aqueous layer is basified with sodium hydroxide and extracted with three 75 ml portions of dichloromethane. Removal of solvent in vacuum affords a residue which when crystallized from heptane gives 3-ethyl-8-benzyl-1-oxa-3,8-diazaspiro[4.5]decan-2-one, mp 105°-106°.
後処理
- temperatureis heated at 90° for one hour
- extractionThe mixture is extracted with two 100 ml portions of hexane
- extractionextracted with three 75 ml portions of dichloromethane
- customRemoval of solvent in vacuum
- customaffords a residue which when
- customcrystallized from heptane
出典と根拠
- ORDレコード
- ord-9e9fd3dfb19e4dd4a035093bee46bbdc
- 出典データセット
- uspto-grants-1981_03
- 特許番号
- US04255432
関連ノート
読み込み中…