反应详情

190 mg of the compound from Example 6 (0.39 mol) and 65 mg of ethyl piperidine-4-carboxylate (0.41 mol) are dissolved in 5.0 ml of dimethylformamide, and 75 mg of diethyl cyanophosphonate (0.43 mol) and 81 μl of triethylamine (59 mg, 0.58 mol) are added. The reaction mixture is stirred at room temperature for 2.5 h, then mixed with ethyl acetate and washed with 5% strength potassium bisulphate solution, saturated sodium bicarbonate solution and saturated sodium chloride. The organic phase is dried over sodium sulphate, the solvent is removed in a rotary evaporator, and the residue is purified by preparative HPLC (eluent: acetonitrile/water, gradient 20:80→95:5). 204 mg (87% of theory) of the title compound are obtained.

1. washwashed with 5% strength potassium bisulphate solution, saturated sodium bicarbonate solution and saturated sodium chloride
2. dry with materialThe organic phase is dried over sodium sulphate
3. customthe solvent is removed in a rotary evaporator
4. customthe residue is purified by preparative HPLC (eluent: acetonitrile/water, gradient 20:80→95:5)