Reaction #1107987

Reaction equation

2,5,6-trichloronicotinonitrile

sulfuric acid

→

2,5,6-Trichloronicotinamide

Conditions

Workup

1. 1
   TemperatureThe reaction mixture was cooled
2. 2
   Otherquenched by the addition of water/ice
3. 3
   FiltrationThe solid was collected by filtration
4. 4
   Otherdried in an oven under reduced pressure
5. 5
   OtherThis resulted in 26 g of 2,5,6-trichloronicotinamide as a white solid

Procedure

A solution of 2,5,6-trichloronicotinonitrile (30 g, 144.92 mmol, 1.00 equiv) in sulfuric acid (98%, 162 mL, 1.00 equiv) was stirred for 1 h at 60° C. in an oil bath. The reaction mixture was cooled and then quenched by the addition of water/ice. The solid was collected by filtration and dried in an oven under reduced pressure. This resulted in 26 g of 2,5,6-trichloronicotinamide as a white solid. LC-MS (ES, m/z): 225 [M+H]+. 1H-NMR (300 MHz, DMSO-d6) δ (ppm) 9.38 (1H, s), 8.12 (1H, s), 7.95 (1H, s).

Source