Reaction #1820156
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07932255B2
Conditions: temp:71.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: To a dry 100.0 ml one necked round bottom flask equipped with a stirring bar is added (S)-1-N-Boc-piperazine-2-carboxylic methyl ester (800 mg, 3.275 mmol) under N2. Anhydrous acetonitrile (20 ml) is added to the flask followed by benzyl chloride (0.38 ml, 3.275 mmol) and triethylamine (1.28 ml, 9.17 mmol). Condenser is then put on to the flask and the reaction mixture is heated at 71° C. for 20 minutes. The reaction mixture is allowed to come to room temperature and concentrated under reduced pressure. It is then diluted with dicholoromethane and washed with water and brine. The organic layer is dried over Na2SO4, filtered and concentrated under reduced pressure. The crude compound is flash column purified using hexane and ethylacetate gradient solvent system to yield 570 mg (52%) of the desired product. Condenser is then put on to the flask to come to room temperature concentrated under reduced pressure It is then diluted with dicholoromethane washed with water and brine The organic layer is dried over Na2SO4 filtered concentrated under reduced pressure purified
Source ID: ord-24fa5f899c16441280329e2f68e43806