3-Fluorobenzoyl chloride → 3-Fluorobenzoyl isothiocyanate
反応式
[S-:1][C:2]#[N:3].[K+].[F:5][C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][CH:14]=1)[C:9](Cl)=[O:10]>CC(C)=O>[F:5][C:6]1[CH:7]=[C:8]([CH:12]=[CH:13][CH:14]=1)[C:9]([N:3]=[C:2]=[S:1])=[O:10]参加物
4
反応条件
- 温度
- 40 °C
実験手順
Potassium thiocyanate (11.03 g, 114 mmol) was suspended in acetone (63.1 mL) and heated to 40° C. under nitrogen atmosphere. To this was added 3-fluorobenzoyl chloride (11.35 mL, 95 mmol), and the resulting mixture was stirred at 50° C. for 6 hours. The heterogeneous mixture was filtered, and the solid was further washed with acetone. The filtrate was concentrated and purified by silica gel chromatography (10% EtOAc/Hexanes as the eluent) to afford 3-fluorobenzoyl isothiocyanate (6.5 g, 37.9% yield) as a light orange oil.
後処理
- filtrationThe heterogeneous mixture was filtered
- washthe solid was further washed with acetone
- concentrationThe filtrate was concentrated
- custompurified by silica gel chromatography (10% EtOAc/Hexanes as the eluent)
出典と根拠
- ORDレコード
- ord-251e2acabe6c440c90124ed683697d72
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09115127B2
反応ノート
読み込み中…