Sodium Azide → (E)-4-(4-azidobut-1-enyl)-1,2-dichlorobenzene
反応式
CS(O[CH2:6][CH2:7]/[CH:8]=[CH:9]/[C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([Cl:17])[CH:11]=1)(=O)=O.[N-:18]=[N+:19]=[N-:20].[Na+]>CN(C=O)C.CCOC(C)=O>[N:18]([CH2:6][CH2:7]/[CH:8]=[CH:9]/[C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([Cl:17])[CH:11]=1)=[N+:19]=[N-:20]参加物
5
実験手順
To a solution of Intermediate 2C (1.3 g, 4.4 mmol) in DMF (7 mL) was added NaN3 (0.86 g, 13 mmol). The reaction mixture was stirred at rt for 16 h. The reaction mixture was diluted with EtOAc (100 mL). The organic layer was washed with 10% aqueous LiCl solution (3×200 mL), dried over Na2SO4 and dried in vacuo. The product was isolated by silica gel chromatography to obtain 570 mg (87% yield) of Intermediate 2D. HPLC/MS (Method C) RT=4.02 min, [M+Na]+ 263.2.
後処理
- washThe organic layer was washed with 10% aqueous LiCl solution (3×200 mL)
- dry with materialdried over Na2SO4
- customdried in vacuo
- customThe product was isolated by silica gel chromatography
出典と根拠
- ORDレコード
- ord-a762d278308440e7ba60d976d6ea8c4f
- 出典データセット
- uspto-grants-2016_02
- 特許番号
- US09249096B2
反応ノート
読み込み中…