Comments (1)
22.06.22
- Set up a dry 50 mL 2-neck flask under N2
- Added KBS14 (396 mg, 1.62 mmol) by solution transfer (10 mL dry THF)
- Added LiAlH4 (2.0 mL, 1 M in THF, 2 mmol, 1.23 equiv.)
- Left stirring from 11.05 am
- TLC'd at 2 pm - indicated completion. Unsure of what produces secondary spot in SM - presumed to be decomposition from SM sample (which was > 1 year old).
30:70 ethyl acetate:pet benz
- Quenched with ethyl acetate (15 mL) and poured over Rochelle's salts (40 mL, sat.) to co-ordinate Al salts
- Extracted with ethyl acetate (4 x 40 mL). Drained light-coloured emulsion into aqueous each time
- Washed with brine (100 mL)
- Dried over MgSO4 and rotovapped
Vial (empty) = 15.5814
Vial (full) = 15.9132
Mass = 331.8 mg
NMR
1H NMR (300 MHz, CDCl3) δ 4.33 (s, 2H), 4.24 (t, 2H), 4.18 (m, 7H)
Some residual ethyl acetate but otherwise mostly clean.
from usyd_phd_eln.
Related Issues (20)
- 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
- HPLC results for various samples (BG_8J, 2022_BG_8B, 2022_BG_8C, CRM3) HOT 4
- KBS13-1 HOT 1
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from usyd_phd_eln.