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885698-82-8

TERT-BUTYL 4-(2-CYANOPROPAN-2-YL)PIPERAZINE-1-CARBOXYLATE synthesis

6synthesis methods
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Yield:885698-82-8 77%

Reaction Conditions:

Stage #1: 1-t-Butoxycarbonylpiperazinewith hydrogenchloride in methanol;diethyl ether;dichloromethane at 0; for 1 h;
Stage #2: sodium cyanide;acetone in water at 20; for 72 h;

Steps:

4.C

To a solution of N-BOC-piperazine (1.06 g) in CH2Cl2/MeOH (20 mL) at 0° C. was added 2M HCl in ether (3.14 mL). After 1 h the solvent was removed in vacuo to give a white solid. This was dissolved in water and NaCN was added (280 mg). To this mixture was added a solution of acetone (420 μL) in water (2 mL). The resultant was stirred at room temperature for 72 h then diluted with water and extracted with ethyl acetate. Combined extracts were dried (Na2SO4), filtered and concentrated to give 4-(cyano-dimethyl-methyl)-piperazine-1-carboxylic acid tert-butyl ester (77%).

References:

US2008/76758,2008,A1 Location in patent:Page/Page column 91