HRID717572

反应详情

EQUATION

反应方程式

HRID 717572 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 2-(4-chloro-6-(pyridin-2-yl)pyrimidin-5-yl)acetaldehyde (600 mg) in dry MeCN (10 mL), methyl hydrazine (181 mg) and sodium acetate (422 mg) were added. The reaction mixture was stirred at room temperature for 3 hours and solvents were removed under reduced pressure. The resulting crude was purified by column chromatography using MeOH/CHCl3 (0.5:9.5) as eluent to afford 1-methyl-5-(pyridin-2-yl)-1,4-dihydropyrimido[4,5-c]pyridazine (350 mg) as white solid. 1H NMR (DMSO-d6): δ 3.41 (s, 3H), 3.93-3.94 (d, 2H), 6.92-6.94 (t, 1H), 7.47-7.51 (m, 1H), 7.94-7.99 (m, 1H), 8.00-8.10 (m, 1H), 8.67-8.69 (d, 2H).

WORKUP

后处理

  1. customsolvents were removed under reduced pressure
  2. customThe resulting crude was purified by column chromatography