Electric Literature of 625-98-9, A common heterocyclic compound, 625-98-9, name is 1-Chloro-3-fluorobenzene, molecular formula is C6H4ClF, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
A solution of 261.1 g (2.0 mol) of 1-chloro-3-fluorobenzene in 2000 ml of dry tetrahydrofuran under nitrogen is cooled to -78. To the solution is added 960 ml (2.4 mol) of 2.5 M n-butyllithium in hexanes over a period of 40 minutes. After stirring for 2.5 hours, a slurry of 155 ml of bromine cooled to -78 is added over 30 minutes and the mixture is stirred for 40 minutes before warming to -10. The reaction is quenched with an aqueous solution of 151.3 g (1.2 mol) of sodium sulfite and 16.0 g (0.4 mol) of sodium hydroxide in 500 ml of water. The organic layer is separated, the solvents are removed at ambient pressure, and the product is distilled at 92-96 (20 mm Hg) to obtain 2-bromo-3-fluoro-chlorobenzene as a colorless oil.
The synthetic route of 625-98-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Novartis AG; US6291523; (2001); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics