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31st October 2013 @ 23:52

According to Althea's method AT-6-4. Spoke to Althea who confirmed the use of sealed tube, not Q-tube. Failed reaction AEW 100-2 may have been a result of a perished seal. 

Procedure:

AT-5 (200 mg, 0.8 mmol, 1.0 equiv.), isopropanol (4 mL) and ammonia (8 mL) were stired in a sealed tube and then heated to 120 ˚C [blast shield in place] for 6 hours (according to AT-6-4). 

Asked colleague to switch the reaction off but unfortunately they forgot and reaction remained stirring for 20 h extra. 

Reaction stopped and solvents removed in vacuo. Crude 1H NMR showed the desired product and also the de-brominated product AEW 100-3-B.

Data:

AEW 100-3 crude proton.pdf
AEW 100-3.zip

Hazard and Risk Assessment:

See: Amination of bromochlorothienopyrimidine (AT-6-4) 

InChi:

InChI=1S/C6H2BrClN2S/c7-4-1-3-5(11-4)6(8)10-2-9-3/h1-2H

to 

InChI=1S/C6H4BrN3S/c7-4-1-3-5(11-4)6(8)10-2-9-3/h1-2H,(H2,8,9,10)

Attached Files
AEW 100-3 crude proton.pdf
AEW 100-3.zip
AEW 100-3-B.png