Sodium Azide → 1-(Azidomethyl)cyclopropanecarbonitrile
反応式
CS(O[CH2:6][C:7]1([C:10]#[N:11])[CH2:9][CH2:8]1)(=O)=O.[N-:12]=[N+:13]=[N-:14].[Na+]>C(N)=O.O.C(OCC)(=O)C.CCOCC>[N:12]([CH2:6][C:7]1([C:10]#[N:11])[CH2:9][CH2:8]1)=[N+:13]=[N-:14]参加物
7
反応条件
- 温度
- 120 °C
実験手順
A stirred mixture of (1-cyanocyclopropyl)methyl methanesulfonate (21.52 mmol, 3.77 g) and sodium azide (43.0 mmol, 2.80 g) in N,N-diemethyl formamide (40 mL) was heated to 120° C. for ˜18 hours. The mixture was allowed to cool and was diluted with water and ethyl acetate. The organic layer was separated, dried over sodium sulphate and concentrated under reduced pressure to give an oil. This oil was taken up in ether and washed with water, dried and concentrated under reduced pressure to give the intermediate 1-(azidomethyl)cyclopropanecarbonitrile (1.8 g) as an oil.
後処理
- temperatureto cool
- customThe organic layer was separated
- dry with materialdried over sodium sulphate
- concentrationconcentrated under reduced pressure
- customto give an oil
- washwashed with water
- customdried
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-4edaa6fcfe994d5b84eba45e5b8b845d
- 出典データセット
- uspto-grants-2012_11
- 特許番号
- US08314091B2
反応ノート
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