反応式
[H-].[Na+].[N+:3]([C:6]1[CH:11]=[CH:10][C:9]([C:12]23[CH2:18][CH:16]([CH2:17]2)[C:15](=[O:19])[NH:14][C:13]3=[O:20])=[CH:8][CH:7]=1)([O-:5])=[O:4].[CH2:21](I)[CH:22]([CH3:24])[CH3:23].C(OCC)(=O)C.CCCCCC>CN(C)C=O>[CH2:21]([N:14]1[C:15](=[O:19])[CH:16]2[CH2:17][C:12]([C:9]3[CH:8]=[CH:7][C:6]([N+:3]([O-:5])=[O:4])=[CH:11][CH:10]=3)([CH2:18]2)[C:13]1=[O:20])[CH:22]([CH3:24])[CH3:23]参加物
実験手順
0.36 g of sodium hydride is added to a solution of 2.46 g of 1-(4-nitrophenyl)-3-azabicyclo[3.1.1]heptane-2,4-dione in 25 ml of N,N-dimethylformamide and the whole is stirred at room temperature for 30 minutes. 2.76 g of isobutyl iodide dissolved in 10 ml of N,N-dimethylformamide are then added dropwise thereto. When the reaction is complete, the reaction mixture is freed of N,N-dimethylformamide. The residue is partitioned between ethyl acetate and water, and the organic phase is dried over magnesium sulphate and, after concentration by evaporation and purification by chromatography over silica gel in the system ethyl acetate/hexane 1:2, the product is obtained in the form of a solid. Melting point 136°-137°. Rf (ethyl acetate/hexane 4:1)=0.6.
後処理
- additionare then added dropwise
- customThe residue is partitioned between ethyl acetate and water
- dry with materialthe organic phase is dried over magnesium sulphate
- concentrationafter concentration
- customby evaporation and purification by chromatography over silica gel in the system ethyl acetate/hexane 1:2
- customthe product is obtained in the form of a solid
出典と根拠
- ORDレコード
- ord-dc11d1a307d54ef491e70b9463a852cc
- 出典データセット
- uspto-grants-1987_06
- 特許番号
- US04677129
関連ノート
読み込み中…