Comments (6)
17.03.22
- cooled 10 mL methanol in ice
- added acetyl chloride (0.4 mL, 5.61 mmol)
- left stirring on ice for 15 mins
- added ferrocencarboxylic acid (1.0031 g, 4.36 mmol)
- warmed to room temperature and began refluxing at 12.30 (heating mantle, condenser, under nitrogen due to humidity)
- turned off after 1 hour of reflux and left to cool
- TLC indicated reaction was not complete
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18.03.22
- heated to reflux again at 10am
- took off at 11am as TLC indicated signs of decomposition (third product appeared below SM spot). Reaction mixture also appeared grainy and darker in colour, as compared to the reddish colour prior to second reflux
- left to crystallise
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23.03.22
- no crystallisation after being left in fridge for multiple days
- quenched with NaHCO3 (50 mL) and NaOH (10 mL) until basic (pH ~ 11)
- rotvapped all methanol off -- runoff was bright yellow and does seem to contain product or an impurity with similar Rf value
- transferred to separating funnel with brine (150 mL) and water (50 mL)
- added 125 mL EtOAc
- separated
- extracted with another 100 mL of EtOAc and left to separate overnight
from usyd_phd_eln.
24.03.22
- 3rd extraction with 100 mL EtOAc
- lots of emulsification -- tried to decant organic layer when pouring off to leave dark brown solid in sep funnel
- 4th extraction with EtOAc (100 mL)
- dried over MgSO4
After addition of MgSo4
from usyd_phd_eln.
29.03.22
- filtered and rotovapped
- vial = 16.0381 g
- vial (product) = 16.7529 g
- product = 0.7148 g
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NMR
1H NMR (300 MHz, Chloroform-d) δ 4.80 (t, J = 2.0 Hz, 2H), 4.39 (t, J = 2.0 Hz, 2H), 4.20 (s, 5H), 3.81 (s, 3H).
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Related Issues (20)
- 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
- 2023_BG_12C
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