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Reaction id: 0501011062_07, verified by Personal Chemistry ©
r3_1
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4c
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DCE
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8a
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Yield: 92% Time: 400s Temperature: 140 °C
Chemicals
| Name |
MW [g/mol] |
Density [g/ml] |
Amount [mmol] |
Mass/Volume |
| 30354-18-8 |
93.557 |
1.000 |
1.496 |
140.000 mg |
| Substrate 1 |
301.364 |
1.000 |
0.664 |
200.000 µl |
| DCE |
98.960 |
1.250 |
37.894 |
3000.000 µl |
| Product 1 |
358.460 |
1.000 |
0.000 |
0.000 µl |
Keywords
Mannich Reaction, C-C coupling
Comments
Synthesis: When attempted using aqueous formaldehyde or paraformaldehyde, this Mannich type reaction gave poor yields, probably due to slow iminium salt formation.
Work-up and purification: After heating, the reaction mixture was diluted with dichloromethane and methanol and then concentrated. The product was purified by column chromatography (silica eluted with ethyl acetate -> 2.5% triethylamine in ethyl acetate).
Characterisation: By refraction index, IR, 1H NMR, 13C NMR and HRMS.
Instrument Settings
Absorption level: Normal
Pre-stirring time: 0s
References
Pemberton, N.; Aaberg, V.; Almstedt, H.; Westermark, A.; Almqvist, F. J. Org. Chem. 2004, 23, 7830-7835
Analysis
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