反应详情

To 13 mL of acetone, there were added 10.04 g of p-nitro-L-phenylalanine and 28 mL of water to thus form a suspension and the latter was cooled in an ice-bath. To this suspension, there were alternatively dropwise added 18.4 mL of a 6M sodium hydroxide solution and 10.05 g of 2,6-dichlorobenzoyl chloride in such a manner that the pH value of the suspension was maintained at a level of not less than 13 at a temperature of not more than 15° C. After the completion of the dropwise addition, the suspension was further stirred for 2 hours with cooling in an ice-bath, then the progress of the reaction was confirmed by HPLC and 36 mL of a 2M hydrochloric acid solution was dropwise added while taking care to prevent any excess generation of heat. The suspension containing separated solid matter was stirred at 10° C. overnight, the precipitates were isolated through filtration and then dried under reduced pressure at 60° C. to thus obtain 17.32 g of the title compound as a white crystalline solid (yield: 95%).

1. customto thus form a suspension
2. temperaturethe latter was cooled in an ice-bath
3. temperaturewas maintained at a level of not less than 13 at a temperature of not more than 15° C
4. additionAfter the completion of the dropwise addition
5. temperaturewith cooling in an ice-bath
6. additionwas dropwise added
7. temperatureof heat
8. additionThe suspension containing
9. customseparated solid matter
10. stirringwas stirred at 10° C. overnight
11. customthe precipitates were isolated through filtration