3,5-difluoro-N-methoxy-N-methylbenzamide synthesis
- Product Name:3,5-difluoro-N-methoxy-N-methylbenzamide
- CAS Number:874889-34-6
- Molecular formula:C9H9F2NO2
- Molecular Weight:201.17
Yield:874889-34-6 100%
Reaction Conditions:
with benzotriazol-1-ol;N-(3-dimethylaminopropyl)-N-ethylcarbodiimide;triethylamine in dichloromethane at 0 - 20;
Steps:
29.b b)
b) 3,5-Difluoro-N-methoxy-N-methyl-benzamide To an ice cooled mixture of 3,5 difluoro benzoic acid (2.0 g, 0.012 mol), 1-hydroxy-benzotriazole (HOBT, 2.5 g, 0.018 mol) and N,O-dimethylhydroxylamine HCl (2.35 g, 0.025 mol) in CH2Cl2(100 mL) was added triethylamine (5.0 mL, 0.036 mol) and followed by addition of 1,3-dimethylamino propyl-3-ethylcarbodiimide (EDC, 3.8 g, 0.019 mol). The mixture was allowed to warm to room temperature and continuously stir overnight. The reaction mixture was added EtOAc (300 mL) and then washed by diluted HCl solution, NaHCO3 and NaCl solution. The organic layer was collected and dried with Mg2SO4 and evaporated. The crude product was purified by column (0-50% EtOAc/Heptane) to give the title compound, 2.6 gm colorless oil. (100%)
References:
US2009/105300,2009,A1 Location in patent:Page/Page column 37
6638-79-5
554 suppliers
$6.00/25g
129714-97-2
142 suppliers
$14.00/1g
874889-34-6
18 suppliers
inquiry
455-40-3
302 suppliers
$10.00/5g
874889-34-6
18 suppliers
inquiry