2,2-Difluoro-5-aminobenzodioxole synthesis
- Product Name:2,2-Difluoro-5-aminobenzodioxole
- CAS Number:1544-85-0
- Molecular formula:C7H5F2NO2
- Molecular Weight:173.12
1645-96-1
1544-85-0
Under nitrogen atmosphere, 2,2-difluoro-5-nitro-1,3-benzodioxolane (69.1, 0.5 g, 2.46 mmol, 1.0 eq.) was dissolved in methanol (3.0 mL) and this solution was added to a 10% palladium/carbon (0.05 g) suspension in methanol (5.0 mL). Subsequently, the reaction system was purged with hydrogen for 2 hours. Upon completion of the reaction, the reaction mixture was filtered through diatomaceous earth and washed with methanol. The collected filtrate was concentrated under reduced pressure to give the crude product. The crude product was purified by n-hexane milling to finally give 2,2-difluorobenzo[d][1,3]dioxolan-5-amine (69.2, 0.31 g, 72.5% yield). Mass spectrum (electrospray ionization): m/z 173.12 [M + H]+.
1583-59-1
250 suppliers
$9.00/5g
1544-85-0
131 suppliers
$15.00/1 g
Yield:-
Steps:
Multi-step reaction with 2 steps
1: nitric acid; sulfuric acid / dichloromethane / 0.5 h / 0 °C
2: potassium carbonate; 5%-palladium/activated carbon; hydrogen / methanol / 4 h / 40 °C / 1500.15 Torr
References:
Li Jinling CN109134442, 2019, A
1645-96-1
54 suppliers
$7.00/1g
1544-85-0
131 suppliers
$15.00/1 g