Hydrochloric Acid → HCID 22416546, compound

Temperature

0 °C

After 6-amino-3-cyanopyridine (1.0 g, 8.4 mmol) was dissolved in 1-propanol (50 ml) and hydrogen chloride gas was passed into the solution at a temperature of 0°-10° C. for 30 minutes, the reactor was tight sealed for stirring the mixture at 0° C. for 21 hours. After the completion of the reaction, the reaction mixture was concentrated under reduced pressure, and a saturated aqueous sodium hydrogen carbonate solution (50 ml) was added to the concentrated mixture to adjust the pH to alkaline. The mixture was extracted with chloroform (50 ml×3). The chloroform layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to give a crude product of propyl 6-amino-3-pyridinecarboximidate (1.56 g).

1. customthe reactor was tight sealed
2. customAfter the completion of the reaction
3. concentrationthe reaction mixture was concentrated under reduced pressure
4. additiona saturated aqueous sodium hydrogen carbonate solution (50 ml) was added to the concentrated mixture
5. extractionThe mixture was extracted with chloroform (50 ml×3)
6. dry with materialThe chloroform layer was dried over anhydrous sodium sulfate
7. concentrationconcentrated under reduced pressure

ORD record

ord-81c3b3a62771448caaf62bbaa941e930

Source dataset

uspto-grants-1996_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05508293