1-Chloro-2-fluoro-4-methylbenzene

colorless and clear liquid

Take 886g compound mixture of formula () and a compound of formula () (3.79mol) 10L into the reaction vessel, put into 8.5L 25% sulfuric acid, was heated to 110 deg.] C to reflux, no starting material the LC track, to stop the reaction, standing layer, Distillation of the organic phase was collected, and 360 g of the compound of the formula (VIII) was collected with purity of 99.0% (2.49 mol) at 156 C.; the purity of the compound 148 g of the formula (IX) was 98.9% (1.02 mol) at 164 C. The results were basically maintained with the analysis result. Consistent.Into 9931g of acetic acid, 2.7g of manganese acetate, 105g98% sulfuric acid to a 20L autoclave, and then put into 99% 3-fluoro-chlorotoluene 870g (5.96mol), stirred mixture was cooled to 15 , ozone slowly into 215g (total 10H); after completion of the reaction of nitrogen with the ozone photodissociation process; temperature and pressure recovery acetate, layers were separated and the product is recovered 988G, to give 3-fluoro-4-chlorobenzoic acid, 98.2% pure, a yield of about 94.2 %.(Step 1) Synthesis of 1-chloro-2-fluoro-4-methyl-5-nitrobenzene 1-Chloro-2-fluoro-4-methylbenzene (1.00 g) was dissolved in TFA (10 mL). The solution was cooled to 0 C., and then, fuming nitric acid (5.0 mL) was added dropwise thereto. The mixture was stirred at 0 C. for 30 minutes, and then, the solution was added to an aqueous sodium bicarbonate solution and neutralized, followed by extraction with chloroform. The extract was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel chromatography (hexane/ethyl acetate) to obtain 1.31 g of the title compound as a white solid.1-hloro-2-fluoro-4-methylbenzene (1.00 g) was dissolved in TFA (10 mL). The solution was cooled to 0C, and then, fuming nitric acid (5.0 mL) was added dropwise thereto. The mixture was stirred at 0C for 30 minutes, and then, the solution was added to an aqueous sodium bicarbonate solution and neutralized, followed by extraction with chloroform. The extract was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel chromatography (hexane/ethyl acetate) to obtain 1.31 g of the title compound as a white solid.General procedure: Morpholine lb (1 .0 mmol), LiHMDS (1 .0M in THF, 1 .5 mL) and fluorobenzene derivative (1 .5 mmol) was mixed and heated. Details regarding the individual reactions are given below.The structure of the compounds is provided in figure 2.; Synthesized from

Molecular Weight:144.57
XLogP3:3
Hydrogen Bond Acceptor Count:1
Exact Mass:144.0142060
Monoisotopic Mass:144.0142060
Heavy Atom Count:9
Complexity:94.9
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes