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Multi-step reaction with 3 steps
1: triethylamine / tetrahydrofuran / 6 h / 20 °C
2: palladium 10% on activated carbon; hydrogen / ethanol / 3 h / 40 °C
3: sodium carbonate; sodium hydroxide / water / 6 h / 20 °C / pH 10 / Cooling with ice
Multi-step reaction with 3 steps
1: triethylamine / tetrahydrofuran / 24 h / 20 °C / Cooling with ice
2: hydrogen; palladium 10% on activated carbon / ethanol / 40 °C
3: aq. buffer / pH 10
With sodium carbonate; sodium hydroxide In water at 20℃; for 6h; Cooling with ice;
In aq. buffer
At first, 27 mmol of carboxyfluorophenylboronic acid (formula (11)) was added with 50 mL of thionyl chloride, and refluxed at 90° C. (degrees Celsius) in an oil bath, and then a solution was produced. Subsequently, the redundant thionyl chloride was removed from the reaction mixture, which was then dissolved in 90 mL of tetrahydrofurane (THF), added with mmol of the compound represented by the above formula (13), further added with triethylamine (TEA) 200 mmol in an ice water bath, and then the mixture was stirred at room temperature for one day.The product solution obtained in this manner was added with a diluted hydrochloric acid solution saturated with sodium chloride salt, and subjected to the procedures for washing and separating the solution, and then THF was removed. The residue was dissolved in 400 mL of ethanol, and added with 1 g of 10% palladium carbon catalyst, and subjected to hydrogen reduction reaction under the condition of 40° C. (degrees Celsius). Then, the palladium carbon catalyst was filtered out therefrom, and the intermediate represented by the formula (15) (FIG. 1) was obtained from the filtrated solution. Subsequently, the obtained intermediate was added with 50 mmol of acryloyl chloride and 150 mL of a buffer solution of a carbonate salt (100 mM, pH 10), and stirred. In this way, sample 1 as a working example was obtained.
With sodium carbonate; sodium hydroxide In water at 20℃; for 6h; Cooling with ice;
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