反応式
[CH3:1][C:2]1[CH:3]([C:10]2[CH:17]=[CH:16][CH:15]=[CH:14][C:11]=2[CH:12]=O)[C:4]([CH3:9])=[C:5]([CH3:8])[C:6]=1[CH3:7].[CH3:18][C:19]1[CH:20]=[C:21]([CH:23]=[C:24]([CH3:26])[CH:25]=1)[NH2:22].C(O)(=O)C.[BH4-].[Na+]>C(O)C.C1(C)C=CC=CC=1.O>[CH3:1][C:2]1[CH:3]([C:10]2[CH:17]=[CH:16][CH:15]=[CH:14][C:11]=2[CH2:12][NH:22][C:21]2[CH:23]=[C:24]([CH3:26])[CH:25]=[C:19]([CH3:18])[CH:20]=2)[C:4]([CH3:9])=[C:5]([CH3:8])[C:6]=1[CH3:7]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 3
実験手順
To a solution of 2-(2,3,4,5-tetramethylcyclopentadienyl)benzaldehyde (15.0 mmol) in ethanol (44.6 mL) were added dropwise 3,5-dimethylaniline (15.8 mmol) and acetic acid (1.5 mmol) under a nitrogen atmosphere. The mixture was stirred at room temperature. After disappearance of the aldehyde was confirmed by gas chromatography, sodium borohydride (19.5 mmol) was added to the solution and reacted at room temperature for 3 hrs. Water and toluene were then added to the reaction mixture. The organic layer was dried and concentrated. The obtained oily substance was purified by silica gel column chromatography to give N-[2-(2,3,4,5-tetramethylcyclopentadienyl)phenylmethyl]-N-(3,5-dimethylphenyl)amine (4.88 g, yield 73.3%) as a yellow oily substance.
後処理
- additionwas added to the solution
- customreacted at room temperature for 3 hrs
- customThe organic layer was dried
- concentrationconcentrated
- customThe obtained oily substance was purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-3e24f844693c410390771f2533932470
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07732643B2
関連ノート
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