Water → N-Methyl-3-(trifluoromethyl)benzamide

A 2M methylamine-THF solution (20 ml) was added to a solution of triethylamine (7 ml) in dichloromethane (70 ml), a solution of 3-(trifluoromethyl)benzoyl chloride (5.0 g) in dichloromethane (30 ml) was added dropwise thereto under ice cooling, followed by stirring at room temperature for 72 hours. The reaction solution was poured into water, followed by extraction with chloroform. The organic layer was washed with saturated aqueous sodium bicarbonate solution and then saturated brine in this order and dried over anhydrous magnesium sulfate, and the solvent was then evaporated under reduced pressure. The residue was dissolved again in ethyl acetate, washed with saturated aqueous sodium bicarbonate solution and then saturated brine in this order, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The resulting solid was washed with diisopropylether, to obtain, as a colorless solid, N-methyl-3-(trifluoromethyl)benzamide (1.34 g).

1. extractionfollowed by extraction with chloroform
2. washThe organic layer was washed with saturated aqueous sodium bicarbonate solution
3. dry with materialsaturated brine in this order and dried over anhydrous magnesium sulfate
4. customthe solvent was then evaporated under reduced pressure
5. dissolutionThe residue was dissolved again in ethyl acetate
6. washwashed with saturated aqueous sodium bicarbonate solution
7. dry with materialsaturated brine in this order, and dried over anhydrous magnesium sulfate
8. customthe solvent was evaporated under reduced pressure
9. washThe resulting solid was washed with diisopropylether

ORDレコード

ord-74200f13a85849c9a1e20e868422464d

出典データセット

uspto-grants-2013_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08377923B2