3-Fluorobenzoyl chloride → 3-Fluorobenzoyl isothiocyanate
반응식
[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]참가 물질
4
반응 조건
- 온도
- 40 °C
실험 절차
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.
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-251e2acabe6c440c90124ed683697d72
- 출처 데이터셋
- uspto-grants-2015_08
- 특허 번호
- US09115127B2
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