Acetonitrile → HCID 23158120, compound

Temperature

80 °C

1 g of 2-fluoro-4-iodo-pyridine and 5 ml of hydrazine monohydrate were dissolved in 6 ml of acetonitrile, and the mixture was stirred at 80° C. for 2 hours, and the solvents were distilled outunder reduced pressure. 5 ml of dimethylformamide and 3 ml of ethyl orthoformate were added to the residues, stirred at 150° C. for 2 hours, cooled down to room temperature and the reaction was stopped after adding water. The products were extracted with chloroform, and after drying with anhydrous sodium sulfate, the solvents were distilled outunder reduced pressure. The obtained residues were washed with ethyl acetate and 680 g of the above compound was obtained as a white solid.

1. distillationthe solvents were distilled outunder reduced pressure
2. addition5 ml of dimethylformamide and 3 ml of ethyl orthoformate were added to the residues
3. stirringstirred at 150° C. for 2 hours
4. temperaturecooled down to room temperature
5. additionafter adding water
6. extractionThe products were extracted with chloroform
7. dry with materialafter drying with anhydrous sodium sulfate
8. distillationthe solvents were distilled outunder reduced pressure
9. washThe obtained residues were washed with ethyl acetate

ORD record

ord-6d2e107c7cf343f584064054f79bd9e5

Source dataset

uspto-grants-2011_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07902369B2