Sodium Azide → 6-Methoxyindan-1-ylmethylazide
반응식
[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]=1참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-f6282e7a29a14888a04a69ec15de3c97
- 출처 데이터셋
- uspto-grants-1990_07
- 특허 번호
- US04939160
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