Sodium borohydride → 2,6-Difluoro-4-(hydroxymethyl)benzonitrile
反応式
[F:1][C:2]1[CH:9]=[C:8]([CH:10]=[O:11])[CH:7]=[C:6]([F:12])[C:3]=1[C:4]#[N:5].[BH4-].[Na+]>CO>[F:1][C:2]1[CH:9]=[C:8]([CH2:10][OH:11])[CH:7]=[C:6]([F:12])[C:3]=1[C:4]#[N:5]参加物
4
実験手順
2,6-Difluoro-4-formylbenzonitrile (1.36 g, 8.13 mmol; see step (ii) above) was dissolved in 25 mL of methanol and cooled on an ice bath. Sodium borohydride (0.307 g, 8.12 mmol) was added in portions with stirring and the reaction was left for 65 min. The solvent was evaporated and the residue was partitioned between diethyl ether and aqueous sodium bicarbonate. The ethereal layer was washed with more aqueous sodium bicarbonate and brine, dried (Na2SO4) and evaporated. The crude product crystallised soon and could be used without further purification.
後処理
- temperaturecooled on an ice bath
- customThe solvent was evaporated
- customthe residue was partitioned between diethyl ether and aqueous sodium bicarbonate
- washThe ethereal layer was washed with more aqueous sodium bicarbonate and brine
- dry with materialdried (Na2SO4)
- customevaporated
- customThe crude product crystallised soon
- customcould be used without further purification
出典と根拠
- ORDレコード
- ord-79369030234b4b8d968d7b38884fa0de
- 出典データセット
- uspto-grants-2010_08
- 特許番号
- US07781424B2
反応ノート
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