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24th August 2016 @ 01:46

Procedure

The ratio between the reactants in this flask was as follows:250mg of 3-bromo-5-chloro-[1,2,4]triazolo[4,3-a]pyrazine(1.07mmol,1equiv.),30.79mg of Pd(dba)2(53.54µmol, 0.05equiv.), 33.21mg of Pd(dba)2(10.71µmol, 0.05equiv.) 109.42mg of piperadine (1.29mmol,126.94mml,  1.2equiv),154.37mg of t-BuONa(1.61mmol, 1.5equiv.),46.68mg of BINAP(74.96µmol,0.07equiv.) The reactants were placed in the flask and purged with argon then 2ml of toluene was added.The mixture was purged with argon again and stirred under argon at room temperature.The reaction will be monitored by TLC

Log

24th Aug

The reaction started at 3:20pm. After an hour, the reaction had almost gone completion according to TLC(25%of EtOAc in petroleum) There was still a small amout of SM so the reaction was left overnight.

25th Aug

The reaction mixure was diluted with 50ml of EtOAc and washed with 10ml of water. The aquaous layer was washed with EtOAc(2x15ml). And the oganic was conbined and concentrated (After working up, TLC looks different)then columned to yield 109mg orange powder. (Yield :43%)

 

 

 

HIRAC

HM 7-1.docx
Attached Files
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HM 7-1.docx
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