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18th August 2016 @ 00:24

Reference:Journal of Medicinal Chemistry, 1979, Vol. 22, No. 11

procedure:

A stirred mixture of 3-bromo-5-chloro-[1,2,4]triazolo[4,3-a]pyrazine (100mg,428.35µmol,1equiv.) and piperazine(33.21mg,385.52µmol,0.9equiv.) was dissolved in 2ml of toluene and kept under N2 at room temperature.The reaction will be monitored by TLC

HIRAC

 

HM 6-1.docx

String:

From 

InChI=1S/C5H2BrClN4/c6-5-10-9-4-2-8-1-3(7)11(4)5/h1-2H

to

InChI=1S/C9H11ClN6/c10-7-5-12-6-8-13-14-9(16(7)8)15-3-1-11-2-4-15/h5-6,11H,1-4H2

Log

18th Aug

The reaction started at 11:30am. The reactant didn't dissolve well in toluene at room temperature.At 1:40TLC was performed with ethyl acetate and petroleum ratio of 1:1, two products appeared.

          

At 3:00pm,TLC was performed again. No obvious change comparing with the former one. The reaction was warmed up to 50℃ and left overnight.

19th Aug

TLC was performed(50%ethyl acetate in petroleum) at 10:00am. No obvious change. The reaction was heated to 110℃

TLC was performed(50%ethyl acetate in petroleum) at 11:30am. No obvious change. Another 0.5 equiv. of piperazine was added.


22th Aug

TLC was performed and the SM was gone. Reaction was switched off.NMR was performed. There might be a peak under the water peak

 

NMR data

Crude NMR(200MHz DMSO)

HM 6-1 crude.png
HM6-1 crude.zip
Attached Files
HM 6-1.png
HM 6-1.docx
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IMG_2764.JPG
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IMG_2782.JPG
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HM 6-1 crude.png
HM6-1 crude.zip