DT A NN-MIXTURE mixture IN-OF of CD-ALPHANUM 124G -LRB- ( CD 150 NN-MASS mg COMMA , CD 0.64 NN-AMOUNT mmol -RRB- ) COMMA , OSCAR-CM 3,5-dichlorobenzylamine -LRB- ( CD 153 NN-MASS mg COMMA , CD 0.87 NN-AMOUNT mmol -RRB- ) CC and OSCAR-CM aluminum OSCAR-CM chloride -LRB- ( CD 27 NN-MASS mg COMMA , CD 0.20 NN-AMOUNT mmol -RRB- ) IN-IN in OSCAR-CM toluene -LRB- ( CD 8 NN-VOL mL -RRB- ) VBD was VB-HEAT refluxed IN-FOR for CD 4 NN-TIME h IN-UNDER under OSCAR-CM nitrogen STOP . IN-AFTER After VB-COOL cooling TO to NN-TEMP room NN-TEMP temperature COMMA , DT-THE the JJ-CHEM reaction NN-CHEMENTITY mixture VBD was VB-TREAT treated IN-WITH with OSCAR-CJ aqueous JJ-CHEM saturated OSCAR-CM NaHCO3 NN-CHEMENTITY solution CC and OSCAR-CM ethylenediaminetetraacetic OSCAR-CM acid -LRB- ( CD 1 NN-MASS g COMMA , CD 3.4 NN-AMOUNT mmol -RRB- ) TO to NN-PH pH CD 7 STOP . DT-THE The NN-CHEMENTITY mixture VBD was VB-EXTRACT extracted IN-WITH with OSCAR-CM chloroform CD four NN-TIMES times STOP . DT-THE The JJ-CHEM combined JJ-CHEM organic NN-CHEMENTITY phases VBD were VB-DRY dried IN-OVER over OSCAR-CM Na2SO4 CC and VB-CONCENTRATE concentrated STOP . DT-THE The NN-CHEMENTITY residue VBD was VB-PURIFY purified IN-BY by JJ preparative NN-CHEMENTITY reverse-phase NNP HPLC TO to VB-YIELD give CD-ALPHANUM 124H STOP .