Triethylamine → 5-Bromo-3-chloro-N-methoxy-N-methylpicolinamide

In N,N-dimethylformamide (24 mL) was dissolved 5-bromo-3-chloropyridine-2-carboxylic acid (2.36 g), 1-hydroxybenzotriazole (2.2 g) and 3-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (2.87 g), N,O-dimethylhydroxylamine hydrochloride (1.27 g) and triethylamine (1.95 mL) was added to the solution, and the resulting mixture was stirred at room temperature for 20 hours. Water was added to the obtained residue, extracted with ethyl acetate, and the organic layer was washed with water and then with a saturated brine. After drying the mixture over anhydrous magnesium sulfate, the mixture was concentrated under reduced pressure to obtain 5-bromo-3-chloro-N-methoxy-N-methylpyridine-2-carboxamide (2.67 g).

1. additionwas added to the solution
2. extractionextracted with ethyl acetate
3. washthe organic layer was washed with water
4. dry with materialAfter drying the mixture over anhydrous magnesium sulfate
5. concentrationthe mixture was concentrated under reduced pressure

ORDレコード

ord-4c13e6800b12474f8e82bf4c7de18409

出典データセット

uspto-grants-2016_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09302996B2