反应详情

温度

90 °C

A mixture of methyl 4-(diethoxyacetyl)-2-fluorobenzoate (0.63 g, 0.0022 mol), thiosemicarbazide (0.24 g, 0.0026 mol), and p-toluenesulfonic acid monohydrate (20 mg) in ethanol (6 mL) was heated at 90° C. for 1.5 h. After cooling to RT, to the mixture was added methyl iodide (0.7 mL, 0.01 mol). The mixture was stirred at RT for 1 h. The mixture was concentrated. The residue was dissolved in acetic acid (4 mL), and heated at 60° C. for 2 h. After cooling, the reaction mixture was concentrated. The residue was treated with methanol. The formed precipitate was collected by filtration, and dried in-vacuo to afford the desired product (180 mg). Analytical LCMS: (M+H)+=280.0.

1. temperatureAfter cooling to RT, to the mixture
2. concentrationThe mixture was concentrated
3. dissolutionThe residue was dissolved in acetic acid (4 mL)
4. temperatureheated at 60° C. for 2 h
5. temperatureAfter cooling
6. concentrationthe reaction mixture was concentrated
7. additionThe residue was treated with methanol
8. filtrationThe formed precipitate was collected by filtration
9. customdried in-vacuo