Sodium Azide → Methyl 4-(azidomethyl)-2-chlorobenzoate
反応式
[N-:1]=[N+:2]=[N-:3].[Na+].[CH3:5][O:6][C:7](=[O:17])[C:8]1[CH:13]=[CH:12][C:11]([CH2:14]Br)=[CH:10][C:9]=1[Cl:16]>CN(C)C=O>[CH3:5][O:6][C:7](=[O:17])[C:8]1[CH:13]=[CH:12][C:11]([CH2:14][N:1]=[N+:2]=[N-:3])=[CH:10][C:9]=1[Cl:16]参加物
4
反応条件
- 温度
- 50 °C
実験手順
Add sodium azide (2.44 g, 37.49 mmol) to crude 4-bromomethyl-2-chloro-benzoic acid methyl ester (7.6 g, 28.84 mmol) in anhydrous dimethylformamide (100 mL) at room temperature under argon gas. Stir the reaction mixture at 50° C. overnight. Quench the reaction mixture with water and extract with ether (3×). Combine the organic layers, wash with brine, dry over sodium sulfate, and concentrate to provide the crude product (5.8 g, 25.7 mmol).
後処理
- customQuench the reaction mixture with water
- extractionextract with ether (3×)
- washCombine the organic layers, wash with brine
- dry with materialdry over sodium sulfate
- concentrationconcentrate
出典と根拠
- ORDレコード
- ord-30dd83ab2ae8426a8bc1992b23881f86
- 出典データセット
- uspto-grants-2010_07
- 特許番号
- US07754742B2
反応ノート
読み込み中…