Methylamine → 3-Bromobenzamide

Temperature

0 °C

To a solution of 3-bromobenzoyl chloride (21.75 g) in THF (20 ml) was added a 40% solution (50 ml) of methylamine in methanol at 0° C. and the mixture was stirred at 0° C. for 1 h. The solvent was evaporated under reduced pressure, and the residue was dissolved in ethyl acetate, the mixture was washed with water and brine, dried (magnesium sulfate) and concentrated under reduced pressure. The residue was recrystallized from ethyl acetate-hexane to give the title compound (18.6 g) as colorless powder crystals.

1. customThe solvent was evaporated under reduced pressure
2. dissolutionthe residue was dissolved in ethyl acetate
3. washthe mixture was washed with water and brine
4. dry with materialdried (magnesium sulfate)
5. concentrationconcentrated under reduced pressure
6. customThe residue was recrystallized from ethyl acetate-hexane

ORD record

ord-684a61684910466eba52dab217fd4342

Source dataset

uspto-grants-2003_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06518257B1