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12th August 2014 @ 06:40

 


AEW 97-10 (50 mg, 0.2 mmol), isopropanol (1.1 mL) and ammonia (aq, 28% (w/w), 2.2 mL) were added to a sealed tube, stirred and heated at 120 °C for 2 hours. TLC showed absense of SM. Volatiles were evaporated and then a crude NMR was run. The yellow solid was purified by adsorbing onto silica and passed through a 10g snap column with dichloromethane and  10% ammonia in MeOH as eluents. Gradient 1-10% NH3/MeOH in CH2Cl2.

Column didn't seem to work terrifically. Three fractions collected and measured on 500 MHz NMR. Second fraction looks promising but NH2 only integrates for 1 and extra peak under A-B system...further investigation required...

Hazard and Risk Assessment:

HIRAC AEW 185-1.doc
HIRAC AEW 185-1.pdf

Data:

AEW 185-1 column frac two 400 MHz.pdf
AEW 185-1 frac one.zip
AEW 185-1 crude.zip
AEW 185-1 frac two.zip
AEW 185-1 frac three.zip

InChi:

InChI=1S/C12H6ClN5/c13-10-6-15-7-11-16-17-12(18(10)11)9-3-1-8(5-14)2-4-9/h1-4,6-7H

to

InChI=1S/C12H8N6/c13-5-8-1-3-9(4-2-8)12-17-16-11-7-15-6-10(14)18(11)12/h1-4,6-7H,14H2

Attached Files
AEW 185-1.cdxml
AEW 185-1.png
HIRAC AEW 185-1.doc
HIRAC AEW 185-1.pdf
aew 185-1_arch.pdf
AEW 185-1 frac one.zip
AEW 185-1 crude.zip
AEW 185-1 frac two.zip
AEW 185-1 frac three.zip
AEW 185-1 column frac one 400 MHz.pdf
AEW 185-1 column frac three 400 MHz.pdf
AEW 185-1 column frac two 400 MHz.pdf
AEW 185-1 crude.pdf