Introduction of a new synthetic route about 2268-05-5

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 2268-05-5, name is 2,6-Dichlorofluorobenzene, A new synthetic method of this compound is introduced below., Safety of 2,6-Dichlorofluorobenzene

To 2,2,6,6-tetramethylpiperidine (20.07 ml_, 1 18 mmol) dissolved in Tetrahydrofuran (THF) (300 ml.) at 0 0C was added nBuLi (73.9 ml_, 118 mmol) dropwise. The solution was stirred at 0 0C for 10 minutes and cooled to -78 0C. 1 ,3- dichloro-2-fluorobenzene (15 g, 91 mmol, commercially available from e.g. Sigma- Aldrich, Apollo or Alfa Aesar) dissolved in Tetrahydrofuran (THF) (30 ml.) was added dropwise and the solution was stirred at -78 0C for 1 hour. The solution was poured on to dry ice (xs) that had been previously washed with tetrahydrofuran (3 x 100 ml.) and stirred to room temperature over 3 hours. Solvents were removed in vacuo to afford a white solid. The solid was combined with solid isolated from method a) and partitioned between ethyl acetate (200 ml.) and 2N Hydrochloric acid. The aqueous solution was extracted with ethyl acetate (3 x 100 ml_); the combined extracts were washed with brine (50 ml.) and concentrated to a crude solid. The crude solid was recrystalised from cyclohexane/toluene to afford the product 19.03 g. LC/MS = 207/209 (M-H)-, retention time = 0.90 minutes (2 minute method).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; GLAXO GROUP LIMITED; DEAN, David Kenneth; MUNOZ-MURIEDAS, Jorge; SIME, Mairi; STEADMAN, Jon Graham Anthony; THEWLIS, Rachel Elizabeth Anne; TRANI, Giancarlo; WALTER, Daryl Simon; WO2010/125102; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics