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Reaction id: 0209191014_01, verified by Personal Chemistry ©
1006
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Pd, 10% on ...
Ammonium fo...
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EtOH
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product 2
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Yield: N/A Time: 180s Temperature: 140 °C
Chemicals
| Name |
MW [g/mol] |
Density [g/ml] |
Amount [mmol] |
Mass/Volume |
| 1148114 |
249.266 |
1.000 |
0.301 |
75.000 mg |
| Ammonium formate |
63.056 |
1.000 |
1.586 |
100.000 mg |
| Pd, 10% on carbon (0.94 mmol/g) |
106.400 |
1.000 |
0.009 |
10.000 mg |
| EtOH |
46.069 |
0.785 |
39.447 |
2315.000 µl |
| Product 1 |
115.132 |
1.000 |
0.000 |
0.000 µl |
Keywords
Deprotection
Comments
Synthesis: Higher temperatures than 140°C did not work due to the high pressure. DMF as solvent did not give any product. MeOH as solvent gave the product and an unidentified by-product. See also entry 0111191011_01 for experimental data.
Work up: 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 pyridine:EtOAc:HOAc:aq 5:5:1:3 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 crude LCMS could be obtained for this product due to its polarity.
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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0209191014_01N_H.pdf