Hydrochloric Acid → HCID 17749871, compound

3.71 g of N-methyl-N-(3-pyridylmethyl)trifluoroacetic acid amide was dissolved in a mixture of 20 ml methanol and 20 ml water, and then stirred with 1.36 g of sodium hydroxide at room temperature for 6 hours. The reaction mixture was made acidic (pH 2) with concentrated hydrochloric acid on ice, and the resulting acidic solution was concentrated under reduced pressure to give a residue. After addition of ethanol, the residue was filtered to remove the precipitated inorganic salts. The filtrate was concentrated under reduced pressure, dried and then recrystallized from methanol/ethanol to give 3-(methylaminomethyl)pyridine dihydrochloride (3.16 g, 95%).

1. concentrationthe resulting acidic solution was concentrated under reduced pressure
2. customto give a residue
3. filtrationthe residue was filtered
4. customto remove the precipitated inorganic salts
5. concentrationThe filtrate was concentrated under reduced pressure
6. customdried
7. customrecrystallized from methanol/ethanol

ORD record

ord-2fe895ff971c4ca29a9b55ad0cd8d012

Source dataset

uspto-grants-2002_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06413995B1