Comments (7)
03.05.22
KBS15 (249 mg, 1.15 mmol) was dissolved in dry THF (13 mL) and DBU (0.21 mL, 1.41 mmol, 1.2 equiv.) and DPPA (0.37 mL, 1.72 mmol, 1.5 equiv.) were added.
The reaction was heated to 60 C and left stirring from 12 pm.
TLC at 5.20 pm indicated reaction was not yet complete.
from usyd_phd_eln.
04.06.22
TLC at 10am indicated reaction was not yet complete. More DBU (86 μL, 0.575 mmol) and DPPA (148 μL, 0.690 mmol) was added
.from usyd_phd_eln.
05.05.22
TLC at 10 am indicated reaction still wasn't complete. Added more DPPA (75 microL, 0.345 mmol, 0.3 equiv.) and DBU (52 microL, 0.345 mmol, 0.3 equiv.) at 11.30 am.
from usyd_phd_eln.
05.05.22
TLC at 10 am indicated reaction still wasn't complete. Added more DPPA (75 microL, 0.345 mmol, 0.3 equiv.) and DBU (52 microL, 0.345 mmol, 0.3 equiv.) at 11.30 am.
from usyd_phd_eln.
09.05.22
Extracted with toluene (3 X 30 mL) -- organic extract was very dark and a black colour emulsion/powder was present.
Washed with brine (60 mL) and dried over MgSO4 before rotovapping.
Vial (empty): 15.4173
Vial (product): 15.7864
Product: 315 mg (1.31 mmol, 114%)
from usyd_phd_eln.
11.05.22
NMR
NMR analysis was unclear. A large, broad and not well-defined peak was present at approximately 4.18, which may be the result of the 3 expected peaks merging together. In #8 (KBS16-2), a similar effect was seen prior to column purification.
KBS16-3 (red) overlaid with known sample KBS16-2 (blue)
from usyd_phd_eln.
17.05.22
Columned crude product with hexane and ethyl acetate. Took a long time to come off with pure hexane, but overshot the mark when swapping to a gradient of 0 - 20% ethyl acetate -- next time try starting on 5% and include a small gradient up to 10% at the end?
Note fraction 3 has both product and impurity
Fractions 1 and 2 rotovapped down.
from usyd_phd_eln.
Related Issues (20)
- KBS43-3 - Nosyl protection of 1,6-diaminohexane HOT 4
- KBS48-1 - Mitsunobu reaction with KBS28 and KBS43 HOT 7
- KBS23-8 - Azidation of 1-naphthylamine HOT 2
- KBS28-9 - Click coupling of 1-azidonaphthalene and propargyl alcohol HOT 6
- KBS49-1 - Mitsunobu reaction with KBS28 and KBS45 HOT 9
- KBS49-2 - Mitsunobu reaction with KBS28 and KBS45 HOT 17
- 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
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