Sodium Azide → 6-Methoxyindan-1-ylmethylazide
反応式
[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH2:7][CH2:8][CH:9]2[CH2:12]OS(C)(=O)=O)=[CH:5][CH:4]=1.[N-:18]=[N+:19]=[N-:20].[Na+]>CS(C)=O>[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH2:7][CH2:8][CH:9]2[CH2:12][N:18]=[N+:19]=[N-:20])=[CH:5][CH:4]=1参加物
4
実験手順
12.8 g (50 mmol) of methanesulphonic acid (6-methoxyindan-1-ylmethyl) ester and 5.2 g (80 mmol) of sodium azide are dissolved in 130 ml of dimethyl sulphoxide and stirred at 80° for 1 hour. The reaction mixture is poured onto ice-water and extracted by shaking with diethyl ether. The organic phases are washed twice with saturated sodium chloride solution, dried over magnesium sulphate and concentrated to dryness by evaporation under reduced pressure. 9.7 g of crude, oily 6-methoxyindan-1-ylmethylazide are obtained as residue.
後処理
- additionThe reaction mixture is poured onto ice-water
- extractionextracted
- stirringby shaking with diethyl ether
- washThe organic phases are washed twice with saturated sodium chloride solution
- dry with materialdried over magnesium sulphate
- concentrationconcentrated to dryness by evaporation under reduced pressure
出典と根拠
- ORDレコード
- ord-f6282e7a29a14888a04a69ec15de3c97
- 出典データセット
- uspto-grants-1990_07
- 特許番号
- US04939160
反応ノート
読み込み中…