3-Cyanopyridine → Nicotinamide

Temperature

87.5 °C

In a four neck round bottom flask fitted with thermowell, agitator and reflux condenser, 3-cyanopyridine (500 g), de-mineralized water (560 g; pH 7.5), ethyl alcohol (56 g) and 40 g of fresh catalyst prepared in Example 1 were charged. The mixture was heated up to 85-90° C. for 4-6 hrs. The completion of reaction was monitored by HPLC. After the completion of reaction the crude product was cooled to 50-60° C. and filtered to separate niacinamide from the catalyst bed. The catalyst bed was washed with de-mineralized water to make catalyst free from hydrolyzed mass of 3-cyanopyridine. The wet catalyst obtained was recycled back for next batch of hydrolysis. The colorless mother liquor was concentrated and dried to get 561.5 g niacinamide. Purity: 99.6% (w/w); niacin content<0.23%; Melting Point: 128-131° C. The water layer recovered containing 3-cyanopyridine and alcohol was recycled back for next hydrolysis batch.

1. customIn a four neck round bottom flask fitted with thermowell, agitator
2. temperaturereflux condenser
3. customThe completion of reaction
4. temperaturewas cooled to 50-60° C.
5. filtrationfiltered
6. customto separate niacinamide from the catalyst bed
7. washThe catalyst bed was washed with de-mineralized water
8. customThe wet catalyst obtained
9. customwas recycled back for next batch of hydrolysis
10. concentrationThe colorless mother liquor was concentrated
11. customdried

ORD record

ord-3b4c8c2b58764641a72b019de8cc4778

Source dataset

uspto-grants-2015_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08952170B2