Water → 2-Pyridinecarboxamide

Temperature

87.5 °C

In a four neck round bottom flask fitted with thermo well, agitator and reflux condenser, 2-cyanopyridine (100 g), de-mineralized water (150 g) isopropyl alcohol (10 g) and chromium oxide-nickel oxide catalyst (1 g) prepared in Example 2 is charged. The mixture is heated up to 85-90° C. for 4-6 h. The completion of reaction is monitored by HPLC. After the completion of reaction the crude product is cooled and filtered to separate picolinamide from the catalyst bed. The catalyst bed is washed with de-mineralized water to make catalyst free from hydrolyzed mass of 2-cyanopyridine. The wet catalyst is recycled back for next batch of hydrolysis. The colorless mother liquor is concentrated and dried to get pure picolinamide. The recovered water layer containing 2-cyanopyridine and alcohol is recycled back for next hydrolysis batch.

1. customIn a four neck round bottom flask fitted with thermo well, agitator
2. temperaturereflux condenser
3. customThe completion of reaction
4. temperatureis cooled
5. filtrationfiltered
6. customto separate picolinamide from the catalyst bed
7. washThe catalyst bed is washed with de-mineralized water
8. customThe wet catalyst is recycled back for next batch of hydrolysis
9. concentrationThe colorless mother liquor is concentrated
10. customdried

ORD record

ord-2ec9e51a89544d37a549383c36df6c2a

Source dataset

uspto-grants-2015_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08952170B2