反応式
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH:6](Cl)[C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.[CH3:17][NH:18][CH2:19][CH2:20][OH:21].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH:6]([C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=2)[N:18]([CH2:19][CH2:20][OH:21])[CH3:17])=[CH:4][CH:3]=1参加物
5
実験手順
A solution of 4,4′-dichlorobenzhydryl chloride (5.20 g, 19.1 mmol) and 2-(methylamino)ethanol (9.0 g, 0.106 mol) in acetonitrile (100 ml) was treated with powdered anhydrous potassium carbonate (10 g) and the resulting mixture was heated under reflux for 4 h. The cooled mixture was filtered and the filtrate was concentrated in vacuo. The residual oil was diluted with ethyl acetate, washed with water and brine and then dried over anhydrous magnesium sulfate. Evaporation of the solvent in vacuo followed by chromatography on silica gel (elution toluene-ethyl acetate 9:1) gave 4.29 g (79%) of the title material as a white solid: mp 49-50° C.
後処理
- temperaturethe resulting mixture was heated
- temperatureunder reflux for 4 h
- filtrationThe cooled mixture was filtered
- concentrationthe filtrate was concentrated in vacuo
- additionThe residual oil was diluted with ethyl acetate
- washwashed with water and brine
- dry with materialdried over anhydrous magnesium sulfate
- customEvaporation of the solvent in vacuo
出典と根拠
- ORDレコード
- ord-ac697e4e425b454cb4cd33cece9939f7
- 出典データセット
- uspto-grants-2001_07
- 特許番号
- US06255496B1
関連ノート
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