4-Chloroaniline → HCID 178446836、化合物
反応式
[CH3:1][CH:2]([CH3:6])[CH2:3][C:4]#[N:5].[Al+3].[Cl-].[Cl-].[Cl-].[Cl:11][C:12]1[CH:18]=[CH:17][C:15]([NH2:16])=[CH:14][CH:13]=1>C1(C)C=CC=CC=1.O>[Cl:11][C:12]1[CH:18]=[CH:17][C:15]([NH:16][C:4](=[NH:5])[CH2:3][CH:2]([CH3:6])[CH3:1])=[CH:14][CH:13]=1参加物
6
実験手順
To a solution of 3-methylbutanenitrile (250 mg, 3.0 mmol) and AlCl3 (400 mg, 3.0 mmol) in toluene (6 mL) was added 4-chloroaniline (383 mg, 3.0 mmol). The resulting solution was stirred at reflux for 2 h, diluted with water, and extracted with EtOAc. The aqueous layer was neutralized with saturated NaHCO3 solution and extracted with EtOAc. The combined extracts were dried over MgSO4, filtered, and concentrated. The crude product (364 mg, 58% yield) was used for the next step without purification.
後処理
- temperatureat reflux for 2 h
- extractionextracted with EtOAc
- extractionextracted with EtOAc
- dry with materialThe combined extracts were dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-e8724d6cb4a9438c9c3eeb94a9b9a95c
- 出典データセット
- uspto-grants-2005_11
- 特許番号
- US06960601B2
反応ノート
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