Ammonia → 4-Amino-3-chloro-2,5,6-trifluoro-pyridine

To 100 ml of acetonitrile was dissolved 20.5 g of 3-chloro-2,4,5,6-tetrafluoropyridine, and 30 ml of 25% aqueous solution of ammonia was added in three portions while the mixture was stirred and cooled with water, and the stirring was continued for another 30 minutes. The solution was concentrated under reduced pressure. After adding 200 ml of chloroform to the solid residue, the solution was washed with 50 ml of distilled water. The chloroform layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure, and the precipitate was collected by filtration to obtain 16.6 g of the title compound as colorless flake crystals.

1. additionwas added in three portions while the mixture
2. concentrationThe solution was concentrated under reduced pressure
3. additionAfter adding 200 ml of chloroform to the solid residue
4. washthe solution was washed with 50 ml of distilled water
5. dry with materialThe chloroform layer was dried over anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. filtrationthe precipitate was collected by filtration

ORD record

ord-dbc485adc440480ab205de7c8415595c

Source dataset

uspto-grants-2000_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06133284