Lithium cyanide → 4-Fluoro-3-iodobenzeneacetonitrile
反応式
Br[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([F:9])=[C:5]([I:10])[CH:4]=1.[C-:11]#[N:12].[Li+]>CN(C=O)C>[F:9][C:6]1[CH:7]=[CH:8][C:3]([CH2:2][C:11]#[N:12])=[CH:4][C:5]=1[I:10]参加物
4
反応条件
- 温度
- 80 °C
実験手順
4-Bromomethyl-1-fluoro-2-iodo-benzene (33.8 g, 107 mMol) was added to 240 mL of a 0.5M solution of lithium cyanide in DMF. The reaction mixture was heated to 80° C. under an atmosphere of dry N2 and stirred overnight at this temperature. The mixture was then cooled to ambient temperature and partitioned between Et2O and 0.1N aqueous NaOH. The Et2O layer was then washed 4 more times with 0.1N aqueous NaOH. The Et2O layer was then dried over MgSO4, fiftered and concentrated under vacuum to give 24.7 9 of the titled compound as a red solid which was used without purification.
後処理
- temperatureThe mixture was then cooled to ambient temperature
- custompartitioned between Et2O and 0.1N aqueous NaOH
- washThe Et2O layer was then washed 4 more times with 0.1N aqueous NaOH
- dry with materialThe Et2O layer was then dried over MgSO4
- concentrationconcentrated under vacuum
出典と根拠
- ORDレコード
- ord-22fa5b1861d54e62ae9224bdd6740f34
- 出典データセット
- uspto-grants-2000_11
- 特許番号
- US06150377
反応ノート
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