HRID2284489

反应详情

EQUATION

反应方程式

HRID 2284489 的结构方程式

PROCEDURE

实验过程

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).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. customquenched by the addition of water/ice
  3. filtrationThe solid was collected by filtration
  4. customdried in an oven under reduced pressure
  5. customThis resulted in 26 g of 2,5,6-trichloronicotinamide as a white solid