Comments (6)
29.11.22
- NaH (157.1 mg, 60% dispersion in mineral oil, 3.93 mmol)
- Washed NaH with pet. benz. (3 x 5 mL)
- Added KBS3-3 (466.9 mg, 1.48 mmol) dissolved in dry DMF (10 mL)
- Added extra NaH (50.8 mg, 1.27 mmol) -- for a total of 5.20 mmol, 3.51 equiv.
- Added 15-crown-ether (0.8 mL, 4.04 mmol, 2.73 equiv.)
- Left stirring at rt from 11.30 am
TLC repeatedly indicated that SM remained. At 4.30 pm, TLC was unclear but seems to have little SM remaining.
- Cooled to 0 C
- Added propargyl bromide (0.5 mL, 80% in toluene, 6.60 mmol, 4.7 equiv.) dropwise
- Left stirring at rt from 4.45 pm
from usyd_phd_eln.
30.11.22
TLC at 9.30 am indicated formation of mono and bis products.
20% ethyl acetate/pet. benz.; from left to right: 17-10, 17-10/starting material co spot, starting material, 17-11/starting material cospot, 17-11
from usyd_phd_eln.
30.11.22
TLC at 5 pm.
Cooled to 0 C and added extra propargyl bromide (0.3 mL, 3.19 mmol, 2.2 equiv.)
from usyd_phd_eln.
01.12.22
TLC at 1.30 pm.
*30% ethyl acetate in pet. benz.*Decided to work up anyway for better comparison with #50.
- Quenched with NH4Cl (20 mL)
- Extracted with toluene (4 x 50 mL)
- Washed with water (5 x 100 mL)
- Washed with brine (125 mL)
- Dried over mag sulphate and rotovapped.
Reaction immediately after quenching
*First extraction - much darker in colour than #50 *
After brine wash
Empty vial: 15.6260
Full vial: 16.1310
Mass: 505 mg
from usyd_phd_eln.
20.12.22
LRMS
Evidence of SM (339.22), mono product (377.23) and bis product (415.25) in a ratio of roughly 10:7:6 i.e. SM = 43%, mono = 30%, bis = 26%.
from usyd_phd_eln.
13.12.22
Column TLCs.
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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