反应详情

184 g of the product of Example 2 is introduced at 20°±2° C. and 66.15 g of copper cyanide and 420 ml of dimethylformamide are added under agitation the whole is heated while distilling the methylene chloride until a temperature of 130° C. is obtained in the reaction medium and then it is maintained for 5 hours under agitation at this temperature. The medium is cooled down to 20°±2° C. under agitation, maintained for 1 hour under these conditions followed by separation and washing with 3×0.3 vol of dimethylformamide. Then 700 ml of pure 22°Be ammonium hydroxide and 700 ml of demineralized water are added to the mixture agitated at 20°±2° C. Agitation is carried out for 1 hour at 20°±2° C. then the whole is cooled down to 0°±5° C., maintained for 1 hour under agitation at 0°±5° C., followed by separating and washing with 2×140 ml of pure 22°Be ammonium hydroxide at 20°±2° C. then with 4×140 ml of demineralized water then drying. Purification is carried out by adding 1105 ml of ethyl acetate then taking to reflux under agitation and then 12.3 g of acticarbon black CX is added. The reaction medium is maintained under agitation under reflux for 30 minutes, then filtered, followed by washing with 3×61 ml of boiling ethyl acetate, concentration under agitation, cooling down under agitation to 0°±2° C. and maintaining under these conditions for 2 hours. Separation, washing with 3×37 ml of ethyl acetate at 0°±2° C. and drying are carried out. In this way 103.7 g of expected product (clear beige powder) is obtained.

1. temperatureis heated
2. distillationwhile distilling the methylene chloride until a temperature of 130° C.
3. customis obtained in the reaction medium
4. temperatureit is maintained for 5 hours under agitation at this temperature
5. temperatureThe medium is cooled down to 20°±2° C. under agitation
6. temperaturemaintained for 1 hour under these conditions
7. customfollowed by separation
8. washwashing with 3×0.3 vol of dimethylformamide
9. additionThen 700 ml of pure 22°Be ammonium hydroxide and 700 ml of demineralized water are added to the mixture
10. temperaturethe whole is cooled down to 0°±5° C.
11. temperaturemaintained for 1 hour under agitation at 0°±5° C.
12. customby separating
13. washwashing with 2×140 ml of pure 22°Be ammonium hydroxide at 20°±2° C.
14. dry with materialwith 4×140 ml of demineralized water then drying
15. customPurification
16. additionby adding 1105 ml of ethyl acetate
17. temperatureto reflux under agitation
18. addition12.3 g of acticarbon black CX is added
19. temperatureThe reaction medium is maintained under agitation
20. temperatureunder reflux for 30 minutes
21. filtrationfiltered
22. washby washing with 3×61 ml of boiling ethyl acetate, concentration under agitation
23. temperaturecooling down under agitation to 0°±2° C.
24. temperaturemaintaining under these conditions for 2 hours
25. customSeparation
26. washwashing with 3×37 ml of ethyl acetate at 0°±2° C.
27. customdrying