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 0.5 M 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 0.1 N aqueous NaOH. The Et2O layer was then washed 4 more times with 0.1 N aqueous NaOH. The Et2O layer was then dried over MgSO4, filtered 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 0.1 N aqueous NaOH
- washThe Et2O layer was then washed 4 more times with 0.1 N aqueous NaOH
- dry with materialThe Et2O layer was then dried over MgSO4
- filtrationfiltered
- concentrationconcentrated under vacuum
出典と根拠
- ORDレコード
- ord-6810f7002a084c7bb6c57ba7bfaf0819
- 出典データセット
- uspto-grants-2001_09
- 特許番号
- US06294552B1
反応ノート
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