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Reaction id: 0503011031_05, verified by Personal Chemistry ©
Acetophenone
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3-Phenylpropylamine
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AcOH
MP-CNBH3
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CH2Cl2
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Product 6
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Yield: 98% Time: 420s Temperature: 110 °C
Chemicals
| Name |
MW [g/mol] |
Density [g/ml] |
Amount [mmol] |
Mass/Volume |
| 98-86-2 |
120.151 |
1.027 |
0.600 |
70.195 µl |
| 2038-57-5 |
135.210 |
0.947 |
0.500 |
71.389 µl |
| MP-CNBH3 (2.4 mmol/g, MP) |
231.171 |
1.000 |
1.250 |
520.833 mg |
| AcOH |
60.052 |
1.050 |
2.500 |
142.981 µl |
| CH2Cl2 |
84.933 |
1.325 |
39.001 |
2500.000 µl |
| Product 1 |
239.362 |
1.000 |
0.500 |
119.681 mg |
Keywords
N-Alkylation, Polymer Supported Reagent, Solid phase reagent, Reductive amination
Comments
Synthesis: The reaction was also performed in THF, but higher conversion was obtained in dichloromethane. Acetylated secondary amine was also formed as a by-product. Increasing the temperature resulted in higher amounts of by-product.
Work-up: The solids were filtered off and washed with 15 mL dichloromethane. The solution was washed with sat. sodium hydrogencarbonate and water, dried with sodium sulphate and concentrated.
Purification: The crude material was purified by chromatography on a Horizon HPFC System using a 12M prepacked silica column with dichloromethane-methanol 18:1 as eluent system.
Characterisation: By 1H-NMR.
Instrument Settings
Absorption level: Normal
Pre-stirring time: 0s
References
Argonaut Technical Note 500 and 510
Analysis
| Method |
Purity |
Files |
| LC-MS |
98 |
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