Comments (4)
04.05.22
1-bromoadamantane (103.6 mg, 0.482 mmol) was placed in a flask under nitrogen by solution transfer (MeCN, 5 mL). SnCl4 (0.14 mL, 1 M in heptane, 0.3 equiv.) and TMSN3 (0.15 mL, 1.14 mmol, 2.3 equiv.) were added and the reaction was left to reflux at 80 C from 1 pm.
from usyd_phd_eln.
05.05.22
TLC at 11 am indicated reaction completion. Took an aliquot of crude reaction mixture to analyse via NMR.
from usyd_phd_eln.
10.05.22
The reaction was quenched with water (15 mL) and then extracted with ethyl acetate (3 x 10 mL) and washed with brine (30 mL). After being dried over MgSO4, solvent was removed by rotary evaporation to give a crystalline yellowish solid.
Vial (empty): 15.8003 g
Vial (product): 15.8825 g
Product: 82.2 mg
Image of solid obtained after rotary evaporation
NMR
NMR analysis seems to indicate some azidoadamantane present, though the peak at 2.15 is largely obscured by acetonitrile (peak at 2.17).
Reaction mixture (red) overlaid with known sample KBS 11-1 (blue)
from usyd_phd_eln.
14.06.22
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Columned KBS11-6 but failed to find any product in fractions. (100% pet. benz. for 5 CV, 0 - 15% EtOAc in pet. benz. for 8 CV)
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Tried columning again and still saw no product. (25% EtOAc in pet. benz. for 10 CV)
Have retained column but unlikely to be able to recover much pure product.
from usyd_phd_eln.
Related Issues (20)
- KBS48-2 - Mitsunobu reaction with KBS28 and KBS43 HOT 15
- KBS44, 52, 53 (Nosyl deprotection) - master page HOT 4
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- 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
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