反应详情

温度

100 °C

A solution of the product of Step 2 (0.30 g, 0.93 mmol) in 1,4dioxane (6 ml) was treated with a solution of guanidine carbonate (0.33 g, 1.86 mmol) and sodium hydroxide (0.1 7 g, 4.1 mmol) in water (2 ml). The mixture was heated at 100° C. for 4 hours. After cooling to room temperature, water was added and the mixture extracted into ethyl acetate (2×). The organic layers were combined and washed with saturated brine, dried (MgSO4) and concentrated in vacuo. The residue was triturated with dichloromethane and the resulting solid filtered to afford the title compound (200 mg, 67%); MS(ES+) m/e 321 [M+H]+.

1. temperatureAfter cooling to room temperature
2. extractionthe mixture extracted into ethyl acetate (2×)
3. washwashed with saturated brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. customThe residue was triturated with dichloromethane
7. filtrationthe resulting solid filtered