Comments (8)
09.08.22
- Dissolved KBS3 (1.00 g, 3.17 mmol) in dry DMF (20 mL)
- Added NaH (1.748 g, 26.9 mmol, 8.5 equiv.)
- Added propargyl bromide (1.00 mL, 10.6 equiv.)
Reaction immediately went a dirty brown dishwater colour.
Within a few minutes, reaction was completely black.
from usyd_phd_eln.
10.08.22
TLC at 11 am indicated reaction was complete.
- Quenched with NH4Cl (40 mL). Make sure to do this DROPWISE
- Diluted with water (60 mL)
- Extracted with toluene (3 x 125 mL)
- Washed with water (5 x 200 mL)
from usyd_phd_eln.
11.08.22
Empty vial: 16.0985
Full vial: 17.2010
Mass: 1.1025 g
from usyd_phd_eln.
12.08.22
Second extraction
Empty vial: 15.8755
Full vial: 16.4060
Mass: 530.5 mg
from usyd_phd_eln.
15.08.22
LRMS
For both:
KBS17-6 cr.pdf
KBS17-6 cr.d.zip
KBS17-6 cr 2nd extract.pdf
KBS17-6 cr 2nd extract.d.zip
from usyd_phd_eln.
25.08.22
Fractions | Empty vial | Full vial | Mass (mg) | Moles | % | Species |
---|---|---|---|---|---|---|
1-12 | 15.8657 | 15.8807 | 15 | 0.038 | - | - |
13-18 | 16.2209 | 16.2943 | 73.4 | 0.187 | - | - |
19-27 | 15.9732 | 15.9892 | 16 | 0.041 | - | - |
28-47 | 16.0098 | 16.0273 | 17.5 | 0.045 | - | - |
Column runoff | 16.1856 | 16.1994 | 13.8 | 0.035 | - | - |
NMR
KBS17-6 column (2nd extract).zip
KBS17-6 column (2nd extract).pdf
None of these seem to have any product. Will try flushing column with 100% ethyl acetate.
from usyd_phd_eln.
26.08.22
Flushed with 100% ethyl acetate (2nd flush, 30-100 over 3 CV, 100 for 9 CV). NMR unclear, but mass spec indicates only SM present (339 is [M+Na]).
KBS17-6 2nd flush.zip
KBS17-6 2nd flush processed.pdf
Mass spec
KBS17-6 2nd flush.pdf
KBS17-6 2nd flush.d.zip
from usyd_phd_eln.
01.09.22
Manual column
~ 15 cm silica
Starting with 200 mL of 5:95 EtOac:hexanes
100 mL 10:90 as above
100 mL 50:50
150 mL straight ethyl acetate
100 mL 10:90 MeOH:DCM
Fractions | Action | Empty vial | Full vial | Mass (mg) | Moles | % Yield |
---|---|---|---|---|---|---|
3-15 | Mono and bis product | 16.0363 | 16.6931 | 656.8 | 1.67 | 53 |
16-19 | Unknown | 15.9959 | 15.9993 | 3.4 | 0.0087 | 0.3 |
20-28 | Unknown | 16.0607 | 16.0638 | 3.1 | 0.0079 | 0.2 |
29 onwards | SM | 15.8642 | 15.9108 | 46.9 | 0.119 | 4 |
Vial after loading sample: 16.1523
from usyd_phd_eln.
Related Issues (20)
- KBS49-2 - Mitsunobu reaction with KBS28 and KBS45 HOT 17
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- KBS50-1 - Nosyl protection of bis(3-aminopropyl)amine HOT 13
- KBS44-2 - Nosyl deprotection of KBS49 HOT 10
- KBS50-2 - Nosyl protection of bis(3-aminopropyl)amine HOT 9
- KBS53-1 - Nosyl deprotection of KBS48 HOT 12
- KBS52-1 - Nosyl deprotection of KBS51 HOT 7
- KBS51-1 - Mitsunobu reaction with KBS28 and KBS50 HOT 10
- KBS53-2 - Nosyl deprotection of KBS48 HOT 9
- KBS48 (pooled) - purification HOT 3
- KBS52-2 - Nosyl deprotection of KBS51 HOT 2
- KBS51-2 - Mitsunobu reaction with KBS28 and KBS50 HOT 5
- KBS22-2 - Linear click coupling of bis-propargyl diaminohexane and azidoadamantane HOT 6
- Carlota's compounds - for purification HOT 2
- KBS22-3 - Linear click coupling of bis-propargyl diaminohexane and azidoadamantane HOT 8
- KBS52-3 - Nosyl deprotection of KBS51 HOT 14
- 2024_BG_A_1 - Formation of benzoyl thioureas HOT 2
- 2024_BG_B_1 - Hydrolysis of benzoyl thioureas HOT 2
- SAR - for future aminothiazoles
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