反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[C:4]([N+:11]([O-:13])=[O:12])[CH:3]=1.[CH3:14][C:15]1([CH3:23])[NH:20][C:19](=[O:21])[CH2:18][C:17](=[O:22])[CH2:16]1.C(N(CC)CC)C.CC(C)(O)C#N>ClCCl>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([CH:18]2[C:17](=[O:22])[CH2:16][C:15]([CH3:23])([CH3:14])[NH:20][C:19]2=[O:21])=[O:7])=[C:4]([N+:11]([O-:13])=[O:12])[CH:3]=1参加物
実験手順
A solution of 4-chloro-2-nitrobenzoyl chloride (4.4 g) in dry dichloromethane (5 ml) was added at 5°-10° C. to a stirred solution of 6,6-dimethylpiperidine-2,4-dione (2.8 g) and triethylamine (2.8 ml) in dry dichloromethane (50 ml) and the mixture was stirred at ambient temperature for 18 hours. Triethylamine (8.4 ml) and acetone cyanohydrin (0.4 ml) were added successively to the solution and the mixture was stirred at ambient temperature for 4 hours. The resulting solution was washed successively with 2N hydrochloric acid (25 ml) and water (3×25 ml), dried over sodium sulphate and evaporated under reduced pressure to give a yellow solid which was recrystallised from acetonitrile to give 3-(4-chloro-2-nitrobenzoyl)-6,6-dimethylpiperidine-2,4-dione (4 g), mp 162°-162.5° C., as a yellow crystalline solid.
後処理
- stirringthe mixture was stirred at ambient temperature for 4 hours
- washThe resulting solution was washed successively with 2N hydrochloric acid (25 ml) and water (3×25 ml)
- dry with materialdried over sodium sulphate
- customevaporated under reduced pressure
- customto give a yellow solid which
- customwas recrystallised from acetonitrile
出典と根拠
- ORDレコード
- ord-cce4e7944be34b27b9fe87c1ed71c64c
- 出典データセット
- uspto-grants-1992_05
- 特許番号
- US05114461
関連ノート
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