反応式
Br[CH2:2][C:3]1[CH:10]=[CH:9][C:6]([C:7]#[N:8])=[CH:5][CH:4]=1.[N-:11]=[N+:12]=[N-:13].[Na+].O>CN1CCN(C)C1=O>[N:11]([CH2:2][C:3]1[CH:10]=[CH:9][C:6]([C:7]#[N:8])=[CH:5][CH:4]=1)=[N+:12]=[N-:13]参加物
5
実験手順
50 g of 4-bromomethylbenzonitrile is dissolved in 350 ml of 1,3-dimethyl-2-imidazolidinone and stirred at 25° for 2 hours with 32.5 g of sodium azide. The mixture is subsequently combined with 500 ml of water under ice cooling, extracted twice with dichloromethane, washed with water, dried over sodium sulfate, concentrated to dryness under vacuum, and chromatographed on silica gel with hexane/ethyl acetate, thus obtaining 39 g of 4-azidomethylbenzonitrile as a colorless liquid.
後処理
- extractionextracted twice with dichloromethane
- washwashed with water
- dry with materialdried over sodium sulfate
- concentrationconcentrated to dryness under vacuum
- customchromatographed on silica gel with hexane/ethyl acetate
出典と根拠
- ORDレコード
- ord-c905a16c14b340969660360c09b93391
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05411982
関連ノート
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