反应详情

4-t-Butyl-3-chloro-6-hydrazinopyridazine (9.5 g, 48 mmol) and dichloroacetic acid (20 ml) were heated in toluene (130 ml) under Dean Stark conditions for 2.5 hours. The toluene was removed and the residue was poured into water to precipitate the product as a brown solid. The product was purified by chromotography on silica gel using 10% ethyl acetate/dichloromethane as eluant to yield a yellow solid (10.4 g, 74%), 1H NMR (250 MHz, CDCl3) δ 1.59 (9H, s, t-Bu), 6.01 (1H, s, CM), 8.37 (1H, s, ArH); MS (ES+) m/e 293 [MH]+.

1. customThe toluene was removed
2. additionthe residue was poured into water
3. customto precipitate the product as a brown solid
4. customThe product was purified by chromotography on silica gel using 10% ethyl acetate/dichloromethane as eluant