反应详情

温度

50 °C

2-Iodopropane (2.0 mL, 20 mmol) was added to a solution of ethyl 2,3-diaminobenzoate (prepared according to the method of WO 97/10219, page 81, Example 51(1)) (3 g, 16.67 mmol) in N,N-dimethylformamide (20 mL), and the solution stirred at 50° C. for 3 hours. The mixture was concentrated under reduced pressure and the residue partitioned between ethyl acetate (200 mL) and water (50 mL), and the layers separated. The organic layer was washed with water (5×50 mL), dried over magnesium sulphate and concentrated in vacuo. The crude product was purified by column chromatography on silica gel using ethyl acetate:pentane (5:95 to 90:10) to afford the title compound as a yellow oil, 1.4 g.

1. customprepared
2. concentrationThe mixture was concentrated under reduced pressure
3. customthe residue partitioned between ethyl acetate (200 mL) and water (50 mL)
4. customthe layers separated
5. washThe organic layer was washed with water (5×50 mL)
6. dry with materialdried over magnesium sulphate
7. concentrationconcentrated in vacuo
8. customThe crude product was purified by column chromatography on silica gel