反应详情

A magnetically stirred solution of 5nitro-1, 10-phenanthroline (2,.01 g, 8.93 mmol) and tin(II) chloride dihydrate (6.05 g, 26.81 mmol) was heated to reflux for 3 h in ethanol (100 mL) and then concentrated in vacuo to give a viscous residue. The residue was treated with concentrated NaOH and then extracted with CHCl3 (3×50 mL). The organic layer was separated, washed with water (2×50 mL) and brine (1×50 mL), dried over anhydrous sodium sulfate, and then concentrated in vacuo to afford 1.08 g (62%) of the amine as a tan solid: m.p. 255-258 C; MS(fab):m/e 196 (MH+).

1. concentrationconcentrated in vacuo
2. customto give a viscous residue
3. extractionextracted with CHCl3 (3×50 mL)
4. customThe organic layer was separated
5. washwashed with water (2×50 mL) and brine (1×50 mL)
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated in vacuo