Dichloroacetyl chloride → HCID 44574295, compound

Temperature

0 °C

To a suspension of 2-amino-5-cyanopyridine (0.500 g, 4.2 mmol) in dry dichloromethane (20 mL) was added triethylamine (0.830 g, 6.3 mmol) and the mixture stirred at 0° C. To the reaction mixture 2,2-dichloroacetyl chloride (0.923 g, 6.3 mmol) was added dropwise and the mixture was stirred at 0° C. for about 1 hour and then at room temperature for 48 hours. The reaction mixture was diluted with dichloromethane (100 mL) and washed with water (150 mL). The organic layer was dried over anhydrous sodium sulfate and concentrated to obtain the crude product, which was purified by column chromatography (silica gel, 25-30% ethyl acetate in petroleum ether as an eluent) to obtain the title compound.

1. stirringthe mixture was stirred at 0° C. for about 1 hour
2. washwashed with water (150 mL)
3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
4. concentrationconcentrated
5. customto obtain the crude product, which
6. customwas purified by column chromatography (silica gel, 25-30% ethyl acetate in petroleum ether as an eluent)

ORD record

ord-e1d769bfedda449797e34c1c0db26b65

Source dataset

uspto-grants-2012_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08314103B2