Comments (6)
24.08.22
- Dissolved product in DCM (15 mL)
- Washed with buffer solution (15 mL of 50 mmol EDTA in ammonium chloride/ammonia buffer, pH 10) + water (10 mL)
- Washed with buffer solution (30 mL, as above)
- Washed with buffer solution (15 mL, as above) and brine (10 mL)
Aqueous layer was turning faintly blue but DCM layer remained stubbornly green.
- Transferred DCM layer to RBF and added 30 mL buffer solution. Heated to 40 C with stirring from 11.30 am
Empty vial: 15.8517
Full vial: 16.4258
Mass: 574.1 mg
from usyd_phd_eln.
26.08.22
NMR
1H NMR (300 MHz, CDCl3) δ 5.30, 3.78, 3.33, 2.59, 2.47, 2.23, 1.79, 1.60, 1.41.
KBS12-2.zip
KBS12-2 processed.pdf
Peak assignation not yet complete, but appears identical (if more concentrated) to previous attempt, KBS12-1.
from usyd_phd_eln.
06.09.22
Rf value
Rf = 0.51 (2.0/3.9) in 10:90 MeOH:DCM
from usyd_phd_eln.
12.09.22
Found a vial labelled "KBS12-2 extra" - applying same process of removing copper using EDTA buffer (product was a green oil/gel).
~ 5 mL DCM and 8 mL EDTA buffer left stirring from 10.50 am
Removed buffer by pipette and added ~5 mL fresh. Repeated this once more then extracted with a sep funnel.
Empty vial: 16.0582
Full vial: 16.1047
Mass: 46.5 mg
from usyd_phd_eln.
19.09.22
Have been trying to "clean up" sample for characterisation via trituration.
KBS12-2 19-09-22_1.zip
KBS12-2 19-09-22 processed.pdf
Still contains impurities at 0.86 and 1.26 - likely either grease or hexane.
from usyd_phd_eln.
LRMS
20210429KBS12-1.d (2).zip
KBS12.pdf
from usyd_phd_eln.
Related Issues (20)
- MTS 2 - MIC and High/Low for MycetOS compounds (duplicate) HOT 6
- KBS17 - master page HOT 1
- VIV2 - MycetOS compounds HOT 1
- TOX1 - MYOS423, 726, 727, 731 HOT 1
- MTS-3 - USYD compounds (triplicate) and York compounds (initial) HOT 7
- TOX-2 - MYOS432, 617 and 619 HOT 1
- TOX-3 - MYOS compounds 423, 432, 617, 619, 726, 727, 731 (duplicate) HOT 1
- VIV-3 - MYOS423, 617, 619. 727 and 731 HOT 4
- MTS-4 - USyd compounds (if needed), York compounds (duplicate) HOT 7
- VIV-5 - MYOS compounds duplicate HOT 1
- VIV-6 - MYOS423, 619, 727, 731 HOT 1
- TOX-4 - Duplicate for compounds 423, 726, 727, 731 HOT 1
- MTS-5 - USyd + U of York + UCL compounds HOT 4
- VIV-7
- VIV-4 - MYOS compounds 423, 617, 619, 727 HOT 1
- MTS-6 - USyd + U of York + UCL compounds HOT 1
- TOX-5 - replicate for 423, 726, 727, 731 HOT 1
- VIV-8
- MTS-7 - USyd repeats + Uni of York / UCL high-low replicates + Uni of York MIC replicates
- TOX-6 - triplicates for USyd compounds MYOS423, 432, 617, 619, 726, 727, 731
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