反应详情

Sodium nitrite (0.298 g, 4.31 mmol) was added to 6-chloro-N4-(2-chlorophenyl)pyrimidine-4,5-diamine (Intermediate AP1) (1 g, 3.92 mmol) in acetic acid (50% Aq, 25 mL) and DCM (25 mL) at room temperature. The resulting solution was stirred at room temperature for 15 minutes. The reaction mixture was separated and the organic phase was washed with water (10 mL), dried (MgSO4) and evaporated to give crude product (0.600 g) that was used without further purification. 1H NMR (400 MHz, CDCl3) δ δ7.52-7.65 (m, 3H), 7.68-7.73 (m, 1H), 8.97 (s, 1H); m/z (ES+), (M+H)+=266.21; HPLC tR=2.33 min

1. customThe reaction mixture was separated
2. washthe organic phase was washed with water (10 mL)
3. dry with materialdried (MgSO4)
4. customevaporated