Methanol → (4,5-Difluoro-2-nitrophenyl)methanol
反応式
[F:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6](O)=[O:7])=[C:4]([N+:12]([O-:14])=[O:13])[CH:3]=1.B.O1CCCC1.CO>C1COCC1>[F:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([CH2:6][OH:7])=[C:4]([N+:12]([O-:14])=[O:13])[CH:3]=1参加物
5
反応条件
- 温度
- 60 °C
実験手順
To a solution of to 4,5-difluoro-2-nitrobenzoic acid (25.9 g) in THF (90 ml), cooled to 0° C., was carefully added borane-tetrahydrofuran complex (319 ml, 1M in THF). After the addition was complete, the mixture was stirred at 60° C. for 3 h. Methanol (150 ml) was added to the mixture at 0° C. and after 10 minutes the mixture was concentrated in vacuo. The residue was poured into water and extracted with ethyl acetate. The organic layer was washed with sat. aq. NaCl, dried (MgSO4), filtered and concentrated in vacuo.
後処理
- additionAfter the addition
- concentrationwas concentrated in vacuo
- additionThe residue was poured into water
- extractionextracted with ethyl acetate
- washThe organic layer was washed with sat. aq. NaCl
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-3154be931743426e9e0a4e705f9b1e44
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08022218B2
反応ノート
読み込み中…