Reaction conditions investigation of the Mannich/lactamization process.
Entry | Nucleophile | Base (1 eq.) | Time (h) | T (°C) | Solvent | Yielda (%) |
---|---|---|---|---|---|---|
1 | CH3NO2 | K2CO3 | 96 | rt | CH3CN | — |
2 | CH3NO2 | — | 48 | rt | — | Complex mixture |
3 | CH3NO2 | — | 18 | 50 | — | 6a, 80 |
4 | CH3NO2 | — | 20 | 50 | — | 6a, 99 |
5 | DMM | — | 17 | 50 | — | 7a, 80 |
6 | Malononitrile | — | 17 | 50 | — | Complex mixture |
7 | Acetylacetone | — | 24 | 50 | — | Complex mixture |
8 | Acetophenone | — | 24 | 50 | — | No reaction |
Isolated yields by chromatography.