反应详情

Under an argon atmosphere, 2.50 g (19.6 mmol) of 2-methyl-5-chloropyridine and 4.38 g (23.5 mmol) of N-(tert-butyloxycarbonyl)-piperazine are dissolved in 50 ml of absolute toluene. Then, 2.26 g (23.5 mmol) of sodium-tert-butylate, 0.37 g (0.59 mmol) of BINAP, and 0.36 g (0.39 mmol) of tris(dibenzylideneacetone)-dipalladium are added, and it is heated for 12 hours to 70° C. After cooling, the reaction mixture is mixed with diethyl ether, washed three times with saturated sodium chloride solution, dried on sodium sulfate, and solvent is removed in a vacuum. The residue is purified by flash chromatography (cyclohexane/ethyl acetate 9:1).

1. temperatureit is heated for 12 hours to 70° C
2. temperatureAfter cooling
3. washwashed three times with saturated sodium chloride solution
4. customdried on sodium sulfate, and solvent
5. customis removed in a vacuum
6. customThe residue is purified by flash chromatography (cyclohexane/ethyl acetate 9:1)