| 93% |
With potassium carbonate; potassium iodide; In N,N-dimethyl acetamide; at 20 - 50℃; for 12h; |
Compound III-2 (1.00g, 2.07mmol) to a suspension of DMA (5ml) of <strong>[40510-81-4]chloromethyl methyl carbonate</strong> (0.483g, 3.10mmol) and potassium carbonate (0.572g, 4.14mmol) , potassium iodide (0.343 g, 2.07 mmol) was added, and the mixture was stirred for 6 hours at 50C. In addition to the reaction mixture, added DMA (1ml) and stirred for 6 hours. The reaction mixture was cooled to room temperature, stirred for 5 minutes at 50 C. was added a DMA (6 ml), and filtered. The obtained filtrate under ice-cooling, was added dropwise 1 mol / L aqueous hydrochloric acid (10ml) and water (4 ml), and stirred for 1 hour. The precipitated solid was collected by filtration, for 3 hours and dried under reduced pressure at 60 , to obtain Compound II-6 (1.10g, 1.93mmol, 93% yield). |
| 93% |
With potassium carbonate; potassium iodide; In N,N-dimethyl acetamide; at 50℃; for 12h; |
To a suspention of Compound III-2 (1.00 g, 2.07 mmol) in DMA (5 ml) were added <strong>[40510-81-4]chloromethyl methyl carbonate</strong> (0.483 g, 3.10 mmol), potassium carbonate (0.572 g, 4.14 mmol) and potassium iodide (0.343 g, 2.07 mmol) and the mixture was stirred at 50C for 6 hours. To the mixture was added DMA (1 ml) and the mixture was stirred for 6 hours. The mixture was cooled to room temperature, DMA (6 ml) was added thereto, and the mixture was stirred at 50C for 5 minutes. The mixture was filtered. To the obtained filtrate were added lmol/L aqueous solution of hydrochloric acid (10 ml) and water (4 ml) and the mixture was stirred for 1 hour.The presipitated solid was filtered and dried under reduced pressure at 60C for 3 hours to obtain Compound II-6 (l.lOg, 1.93 mmol, 93%).1H-NMR (DMSO-D6) d: 2.91-2.98 (1H, m), 3.24-3.31 (1H, m), 3.44 (1H, t, J = 10.4 Hz), 3.69 (1H, dd, J = 11.5, 2.8 Hz), 3.73 (3H, s), 4.00 (1H, dd, J = 10.8, 2.9 Hz), 4.06 (1H, d, J = 14.3 Hz), 4.40 (1H, d, J = 11.8 Hz), 4.45 (1H, dd, J = 9.9, 2.9 Hz), 5.42 (1H, dd, J = 14.4, 1.8 Hz), 5.67 (1H, d, J = 6.5 Hz), 5.72-5.75 (3H, m), 6.83-6.87 (1H, m), 7.01 (1H, d, J = 6.9 Hz), 7.09 (1H, dd,J = 8.0, 1.1 Hz), 7.14-7.18 (1H, m), 7.23 (1H, d, J = 7.8 Hz), 7.37-7.44 (2H, m). |
| 90% |
With potassium carbonate; potassium iodide; at 50℃; for 12h; |
To a suspension of compound (V) (1.00 g, 2.07 mmol) in DMA (5 ml)Chloromethyl methyl carbonate(0.483 g, 3.10 mmol) and potassium carbonate (0.572 g, 4.14 mmol) and potassium iodide (0.343 g, 2.07 mmol)The temperature was raised to 50 C. and the mixture was stirred for 6 hours. Further, DMA (1 ml) was added to the reaction solution, and the mixture was stirred for 6 hours. The reaction solution was cooled to room temperature,DMA (6 ml) was added and the mixture was stirred at 50 C. for 5 minutes and filtered. 1 mol / L hydrochloric acid water (10 ml) and water (4 ml) were added dropwise to the obtained filtrate under ice cooling, and the mixture was stirred for 1 hour. The precipitated solid was collected by filtration and dried under reduced pressure at 60 C. for 3 hours to obtain the compound (VI) (1.10 g, 1.93 mmol, yield 93%). |
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