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Reaction id: 0210141016_05, verified by Personal Chemistry ©
1187
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Ammonium fo...
Pd, 10% on ...
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EtOH
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product 5
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Yield: N/A Time: 180s Temperature: 140 °C
Chemicals
| Name |
MW [g/mol] |
Density [g/ml] |
Amount [mmol] |
Mass/Volume |
| 66845429 |
380.441 |
1.000 |
0.302 |
115.000 mg |
| Pd, 10% on carbon (0.94 mmol/g) |
106.400 |
1.000 |
0.009 |
10.000 mg |
| Ammonium formate |
63.056 |
1.000 |
1.586 |
100.000 mg |
| EtOH |
46.069 |
0.785 |
39.873 |
2340.000 µl |
| Product 1 |
246.307 |
1.000 |
0.000 |
0.000 mg |
Keywords
Deprotection
Comments
Synthesis: Higher temperatures than 140°C are not recommended due to the obtained pressure during these reactions. Full conversion was reached after 180 s and therefore a longer reaction time will not be necessary. See also e g entry 0111191011 and/or 0209181023 for experimental data.
Work-up: The residue was collected as a slightly blue gel which could be "solved" by adding a few ml of water before filtration. The residue was filtered to remove the catalyst and then concentrated. The compound was collected as white crystals.
Analysis: NMR was performed using DMSO:D2O 5:1 as solvent.
TLC was performed using n-BuOH:EtOAc:HOAc:aq 1:1:1:1 as mobile phase, charring with ninhydrine. Results from TLC confirms full conversion due to no UV absorption, which would be expected from the starting material.
No reliable purity could be obtained from LCMS for this product.
Instrument Settings
Absorption level: Normal
Pre-stirring time: 0s
References
Larsson, U.; Carlson, R. Acta Chem. Scand. 1994, 48 (6), 511-516
Analysis
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0210141016_05N_H.pdf