反应详情

To a suspension of 10.2 g. (28.0 mmol) of 1-(2',6'-dimethylphenyl)-3-[(2-pyridyl)methyl]amidinourea in CH3CN (100 ml) is added 10.0 g. (84.0 mmol) of DMF-DMA and the reaction mixture heated at reflux for two hours. The solvent is removed under vacuum and the residue diluted with H2O and made basic with 10% aqueous NaOH (pH10). The aqueous layer is extracted with CHCl3 (2×100 ml.) and the extracts dried (MgSO4) and concentrated under vacuum to an orange oil, which by NMR looks to be a mixture of starting material and product. The oil is layered out with H2O and Et2O. The oil solidifies. This solid is filtered and washed with H2O and Et2O and air dried. The solid is then crystallized (2×) from EtoAc to give 3.2 g. (37%) of tan crystalline solid, melting point 165°-6° C.

1. additionTo a suspension of 10.2 g
2. temperatureat reflux for two hours
3. customThe solvent is removed under vacuum
4. additionthe residue diluted with H2O
5. extractionThe aqueous layer is extracted with CHCl3 (2×100 ml.)
6. dry with materialthe extracts dried (MgSO4)
7. concentrationconcentrated under vacuum to an orange oil, which by NMR
8. additiona mixture of starting material and product
9. filtrationThis solid is filtered
10. washwashed with H2O and Et2O and air
11. customdried
12. customThe solid is then crystallized (2×) from EtoAc
13. customto give 3.2 g