反应详情

Compound (II) obtained in the previous example (395.0 g, 2.405 mol) and acetone (1074 mL) were placed in a 5 L glass reactor and deionised water (1303 mL) was added to the slightly cloudy resulting solution, with a slight exothermic reaction of 6° C. being observed. Then, Na2CO3 (153.0 g, 1.443 mol) was added, with a slight exothermic reaction of 2° C. being observed. The resulting whitish suspension was cooled with an ice water bath at 0°-5° C. and, for approximately 1 hour without exceeding 5° C., a solution made up of chloroacetyl chloride (III) (201.0 mL, 285.3 g, 2.526 mol) in acetone (735 mL) was slowly added. The addition created vapours and a slight release of gases. The resulting milky suspension was stirred at 0°-5° C. and, after 1.5 hours, Na2CO3 (30.6 g, 0.289 mol) and a solution made up of chloroacetyl chloride (38.3 mL, 54.3 g, 0.481 mol) in acetone (140 mL) was added. After a further 1.5 hours, the suspension was concentrated at reduced pressure to a volume of approximately 1.0 L, with approximately 3.0 L having been distilled. The white thick suspension was cooled to 18°±2° C. and was filtered, with the filter being washed with deionised water (300 mL). A white solid was obtained that was dried at 60° C. and at reduced pressure and, which corresponded to the title product (I), having a melting point of 192-194° C. (483.7 g, 83.55% yield).

1. customwere placed in a 5 L glass reactor
2. temperatureThe resulting whitish suspension was cooled with an ice water bath at 0°-5° C. and, for approximately 1 hour
3. customwithout exceeding 5° C.
4. additionwas slowly added
5. additionThe addition
6. additionwas added
7. waitAfter a further 1.5 hours
8. concentrationthe suspension was concentrated at reduced pressure to a volume of approximately 1.0 L, with approximately 3.0 L
9. distillationhaving been distilled
10. temperatureThe white thick suspension was cooled to 18°±2° C.
11. filtrationwas filtered, with the filter
12. washbeing washed with deionised water (300 mL)
13. customA white solid was obtained
14. customthat was dried at 60° C. and at reduced pressure and, which