反应详情

温度

-5 °C

To a 5000 mL beaker, 1700 mL of water was added and then 11 g of sodium hydroxide was added, followed by stirring to dissolve the sodium hydroxide completely. Then, 26.9 g of 12-aminododecanoic acid (produced by Wako Pure Chemical Industries, Ltd.) was added to the reaction system, followed by stirring for 30 minutes to obtain a homogeneous solution. Subsequently, the internal temperature of the reaction system was cooled to −5° C. with an ice-salt bath. After the cooling treatment, 14.3 g of methacryloyl chloride (produced by Wako Pure Chemical Industries, Ltd.) was dropped over 15 minutes with a dropping funnel while stirring the reaction system. During the dropping, cooling was continued so that the internal temperature of the reaction system might not exceed 0° C. After the end of the dropping, the bath was changed to an ice bath and the reaction system was stirred at 0° C. for 1 hour. After stirring for 1 hour, a 6 mol/L aqueous hydrochloric acid solution was added to adjust the pH of the reaction solution at 3 or less. With the addition of the aqueous hydrochloric acid solution, white precipitate formed in the reaction system. To the solution was added 600 g of sodium chloride, and then extraction was carried out three times using 800 mL of ethyl acetate. The resulting ethyl acetate solution was washed with saturated aqueous sodium chloride solution and then magnesium sulfate was added to the ethyl acetate layer to dehydrate it. After the dehydration, ethyl acetate was distilled off under reduced pressure with a rotary evaporator to give white crude crystals. The resulting crude crystals were recrystallized from ethyl acetate to give 24 g of white crystals of N-methacryloyl-12-aminododecanoic acid (melting point: 73 to 74° C.). The chemical reaction formula of this Example is shown below.

1. stirringby stirring for 30 minutes
2. customto obtain a homogeneous solution
3. stirringwhile stirring the reaction system
4. temperatureDuring the dropping, cooling
5. customexceed 0° C
6. customAfter the end of the dropping, the bath was changed to an ice bath
7. stirringthe reaction system was stirred at 0° C. for 1 hour
8. stirringAfter stirring for 1 hour
9. customformed in the reaction system
10. extractionextraction
11. washThe resulting ethyl acetate solution was washed with saturated aqueous sodium chloride solution
12. additionmagnesium sulfate was added to the ethyl acetate layer
13. distillationAfter the dehydration, ethyl acetate was distilled off under reduced pressure with a rotary evaporator
14. customto give white crude crystals
15. customThe resulting crude crystals were recrystallized from ethyl acetate