Comments (6)
20.09.22
- Added NaH (105 mg, 2.63 mmol, 1.89 equiv.) to a flask under nitrogen
- Added KBS3-3 (1.39 mmol) via solution transfer (15 mL dry THF, 1 mL dry DMF)
- Left stirring from 4.40 pm
- Added propargyl bromide (0.4 mL, 80% in toluene, 4.26 mmol, 3.1 equiv.) at 6.10 pm ON ICE
- Left stirring in ice bath
from usyd_phd_eln.
21.09.22
Removed ice bath (by now a water bath) and TLC'd.
TLC indicated that bis product was forming slowly. Left to keep reacting.
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23.09.22
TLC not much different to Wednesday. Added 0.25 mL propargyl bromide and left stirring.
from usyd_phd_eln.
26.09.22
TLC indicated completion at 10 am, added 50 mL NH4Cl solution to quench and left stirring until 3pm.
Then:
- extracted with toluene (3 x 50 mL)
- washed with water to remove DMF (5 x 100 mL)
- washed with brine (100 mL)
- dried over MgSO4
Crude product
Empty vial: 16.1950
Full vial: 16.6136
Mass: 418.6 mg
H NMR
KBS17-8 cr_1.zip
KBS17-8 cr processed.pdf
Again, appears to have both mono and bis products present.
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LRMS
B
D
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Column details
Manual column run on ~11 cm silica with ethyl acetate/petroleum benzine.
5% - 150 mL
10% - 300 mL
50% - 100 mL
100% - 100 mL
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Related Issues (20)
- KBS48-2 - Mitsunobu reaction with KBS28 and KBS43 HOT 15
- KBS44, 52, 53 (Nosyl deprotection) - master page HOT 4
- KBS50-1 - Nosyl protection of bis(3-aminopropyl)amine HOT 13
- KBS44-2 - Nosyl deprotection of KBS49 HOT 12
- KBS50-2 - Nosyl protection of bis(3-aminopropyl)amine HOT 9
- KBS53-1 - Nosyl deprotection of KBS48 HOT 13
- 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 11
- 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 16
- 2024_BG_A_1 - Formation of benzoyl thioureas HOT 2
- 2024_BG_B_1 - Hydrolysis of benzoyl thioureas HOT 2
- SAR - for future aminothiazoles
- 2024_BG_C - characterisation of final compounds HOT 6
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