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The (R) -3_ (tert-butoxycarbonyl) piperidine-1-carboxylate was dissolved in DMF at 0_5 C, 60% sodium hydride suspension processing. The reaction mixture was warmed to room temperature lOmin, then cooled again, and a solution of 3-bromo-piperidine-1-carboxylate. After 2 hours, warmed to room temperature, an additional amount of 3-bromo-piperidine-1-carboxylate, and the reaction mixture was stirred for 16 hours. The reaction mixture was evaporated under vacuum to ~ 1/4 volume, and partitioned between ethyl acetate and water. The organic solution was then washed with brine phase portions, dried over anhydrous magnesium sulfate, filtered, and evaporated in vacuo to give a residue.
The (R) - 3 - (tert-butoxycarbonylamino) piperidine-1-carboxylic acid benzyl ester in 0-5 C is soluble in DMF, use of sodium hydride 60% suspension processing. The reaction mixture is heated to room temperature 10 min, and then again cooling, and adding 3-bromo piperidine-1-carboxylic acid T-butyl ester. 2 hours later, the temperature is increased to room temperature, adding extra amount of 3-bromo piperidine-1-carboxylic acid T-butyl ester, and stirring the reaction mixture 16 hours. Then the reaction mixture is vacuum evaporation to -1/4 volume, and allocated between the ethyl acetate and water. Then the organic phase part of the salt water solution for washing, drying with anhydrous magnesium sulfate, filtration, and vacuum evaporation to obtain the residue. The residue is dissolved in ethanol, with 10% palladium-carbon processing, and in 60-70psi hydrogenated hydrogen 6.5 hours. The crude reaction mixture is then filtered using diatomaceous earth, vacuum evaporation, and once again is soluble in ethanol, the filtration in order to remove the residual catalyst. Evaporating the mixture, ethyl acetate/hexane on a silica gel chromatography to obtain the title compound (formula: C 20 H 37 N 3 O 4).
The (R) - 3 - (tert-butoxycarbonylamino) piperidine-1-carboxylic acid benzyl ester in 0-5 C is soluble in DMF, use of sodium hydride 60% suspension processing. The reaction mixture is heated to room temperature 10 min, and then again cooling, and adding 3-bromo piperidine-1-carboxylic acid T-butyl ester. 2 hours later, the temperature is increased to room temperature, adding extra amount of 3-bromo piperidine-1-carboxylic acid T-butyl ester, and stirring the reaction mixture 16 hours. Then the reaction mixture is vacuum evaporation to -1/4 volume, and allocated between the ethyl acetate and water. Then the organic phase part of the salt water solution for washing, drying with anhydrous magnesium sulfate, filtration, and vacuum evaporation to obtain the residue.
The (R) - 3 - (tert-butoxycarbonylamino) piperidine-1-carboxylic acid benzyl ester in 0-5 C is soluble in DMF, use of sodium hydride 60% suspension processing. The reaction mixture is heated to room temperature 10 min, and then again cooling, and adding 3-bromo piperidine-1-carboxylic acid T-butyl ester. 2 hours later, the temperature is increased to room temperature, adding extra amount of 3-bromo piperidine-1-carboxylic acid T-butyl ester, and stirring the reaction mixture 16 hours. Then the reaction mixture is vacuum evaporation to -1/4 volume, and allocated between the ethyl acetate and water. Then the organic phase part of the salt water solution for washing, drying with anhydrous magnesium sulfate, filtration, and vacuum evaporation to obtain the residue.The residue is dissolved in ethanol, with 10% palladium-carbon processing, and in 60-70psi hydrogenated hydrogen 6.5 hours. The crude reaction mixture is then filtered using diatomaceous earth, vacuum evaporation, and once again is soluble in ethanol, the filtration in order to remove the residual catalyst. Evaporating the mixture, ethyl acetate/hexane on a silica gel chromatography to obtain the title compound (formula: C20H37N3O4).
The (R) -3- (tert-butoxycarbonyl) piperidine-1-carboxylate was dissolved in DMF at 0-5 , with sodium hydride 60% dispersion treatment. The reaction mixture was warmed to room temperature 10min, then cooled again, and a solution of 3-bromo-piperidine-1-carboxylate. After 2 hours, warmed to room temperature, an additional amount of 3-bromo-piperidine-1-carboxylate, and the reaction mixture was stirred for 16 hours. The reaction mixture was evaporated in vacuo and then to ~ 1/4 volume and partitioned between ethyl acetate and water. The organic portion was washed with brine solution, dried over anhydrous magnesium sulfate, filtered, and evaporated in vacuo to give a residue. The residue was dissolved in ethanol, treated with 10% palladium on carbon and hydrogen for 6.5 hours at 60-70psi. The crude reaction mixture was filtered through celite, evaporated in vacuo, and dissolved again in ethanol, filtered to remove catalyst residues. The mixture was evaporated and chromatographed on silica gel using ethyl acetate / hexane to obtain the title compound (molecular formula: C20H37N3O4).
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