反应详情

To a solution of 4-benzyloxycarbonyl-1-[3-(benzhydrylidene-amino)-4-cyano-benzyl]-3-(S)-(2-methylsulfanyl-ethyl)-piperazin-2-one (1.17 g, 2.67 mmol) in 15 ml of ethanol is added 1,3,5-triazine and glacial acetic acid (3.1 ml, 53.4 mmol). The resulting solution is refluxed for 20 hours, concentrated under vacuum. The residue is dissolved in ethyle acetate, washed with 1N hydrochloric acid, a saturated aqueous NaHCO3 solution, water, brine. The solution is dried over MgSO4, concentrated. The resulting crude product is purified by column chromatography eluting with a gradient of 5% MeOH:CH2Cl2 to 10% MeOH:CH2Cl2. The title compound (489 mg, 39% yield) is obtained as a yellow solid.

1. temperatureThe resulting solution is refluxed for 20 hours
2. concentrationconcentrated under vacuum
3. dissolutionThe residue is dissolved in ethyle acetate
4. washwashed with 1N hydrochloric acid
5. dry with materialThe solution is dried over MgSO4
6. concentrationconcentrated
7. customThe resulting crude product is purified by column chromatography
8. washeluting with a gradient of 5% MeOH