HRID1178927

反应详情

EQUATION

反应方程式

HRID 1178927 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Add concentrated HCl (0.46 mL) to a suspension 2-fluoro-nicotinonitrile (0.34 g, 2.8 mmol) and 5% Pd/C (0.5 g) in methanol (10 mL) at RT. Stir suspension under an atmosphere of hydrogen at 1 atm. For 6 hours. Filter reaction mixture and concentrate the filtrate. Add ether to the residue, bubble HCl gas through the suspension, filter precipitate, and dry to give the title compound (0.37 g, 82%). MS (ES) 127.1 (M+1)+. 1H NMR (400 MHz, DMSO) δ: 8.65 (brs, 3H), 8.24 (m, 1H), 8.16 (m, 1H), 7.41 (m, 1H), 4.06 (m, 2H).

WORKUP

后处理

  1. filtrationFilter
  2. customreaction mixture
  3. concentrationconcentrate the filtrate
  4. customAdd ether to the residue, bubble HCl gas through the suspension
  5. filtrationfilter precipitate
  6. customdry