Sodium Carbonate → HCID 23721152, compound

A dried flask made of Pyrex glass (capacity of 500 ml) provided with a reflux condenser was charged with an inert gas to purge the air from theflask. Then, metallic magnesium (4.65 g) and anhydrous diethyl ether (100 ml) were fed to the flask, and the resulting solution was stirred and cooled by ice bath. A solution prepared separately by adding anhydrous diethylether (50 ml) to 1-bromo-3,5-difluorobenzene (43.52 g) was added dropwise thereto over one hour, and the resulting solution was left still for three hours. At the end of the reaction, a liquid containing boron trifluorideethercomplex (4.542 g) in anhydrous diethyl ether was added dropwise over 40 minutes, and left still for 16 hours with stirring at the room temperature. Then, an aqueous solution of sodium carbonate (30 g) in pure water (100 g) was dropped with 30 minutes. After the solution was kept stirring at the room temperature for 24 hours, the water phase and the organic phase were separated from each other. The separated organic phase was dried with sodium sulfate and filtered; the filtrate was put into an evaporator (oil bath temperature: 70° C.); and diethyl ether was evaporated, thereby obtaining a liver-brown colored solid. The liver-brown colored solid was further purified with silica gel, and a white solid of tetrakis(3,5-difluorophenyl)borate sodium salt (10.3 g) was obtained.

1. customA dried flask made of Pyrex glass (capacity of 500 ml)
2. customprovided with a reflux condenser
3. additionwas charged with an inert gas
4. customto purge the air from theflask
5. temperaturecooled by ice bath
6. customA solution prepared separately
7. additionwas added dropwise
8. waitthe resulting solution was left still for three hours
9. customAt the end of the reaction
10. additionwas added dropwise over 40 minutes
11. waitleft still for 16 hours
12. stirringwith stirring at the room temperature
13. stirringAfter the solution was kept stirring at the room temperature for 24 hours
14. customthe water phase and the organic phase were separated from each other
15. dry with materialThe separated organic phase was dried with sodium sulfate
16. filtrationfiltered
17. customthe filtrate was put into an evaporator (oil bath temperature: 70° C.)
18. customand diethyl ether was evaporated
19. customobtaining a liver-brown colored solid
20. customThe liver-brown colored solid was further purified with silica gel

ORD record

ord-916758221a404253a4bc14fe5b649203

Source dataset

uspto-grants-2002_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06387975B1