HRID1059685

反应详情

EQUATION

反应方程式

HRID 1059685 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A stirred solution of 6.11 g (50.1 mmol) of 2-cyano-3-fluoropyridine in 250 mL of ethanol and 12.5 mL (150 mmol) of conc. HCl was hydrogenated over 1.90 g of 10% palladium on carbon at 40 psi for 16 h. The catalyst was removed by filtration and the solvents removed at reduced pressure. The resulting solid was diluted with acetonitrile and filtered to give 8.0 g of A as an off-white solid: 1H NMR (CD3OD) δ 8.48 (d, 1H, 4.8 Hz), 7.69 (td, 1H, 9.2, 1.1 Hz), 7.68 (ddd, 1H, 8.8, 4.4, 4.4 Hz), 4.34 (s, 2H).

WORKUP

后处理

  1. customThe catalyst was removed by filtration
  2. customthe solvents removed at reduced pressure
  3. additionThe resulting solid was diluted with acetonitrile
  4. filtrationfiltered
  5. customto give 8.0 g of A as an off-white solid