1,1-Dichloroethane → Chloromethyl 3-fluorobenzoate

To 10 ml of dichloroethane were added 1.32 g of zirconium tetrachloride and 1 g of 3-fluorobenzoyl chloride, and the mixture was stirred at room temperature for 20 minutes. The mixture was cooled to 0° C., 0.21 g of trioxane was added, and the mixture was stirred for 1 hour, and further stirred at room temperature for 1 hour. Water was added slowly at 0° C., the resultant solution was extracted with chloroform three times, and the organic layers were combined, washed with an aqueous saturated sodium bicarbonate solution and an aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated to obtain 0.65 g of chloromethyl 3-fluorobenzoate.

1. temperatureThe mixture was cooled to 0° C.
2. stirringthe mixture was stirred for 1 hour
3. stirringfurther stirred at room temperature for 1 hour
4. extractionthe resultant solution was extracted with chloroform three times
5. washwashed with an aqueous saturated sodium bicarbonate solution
6. dry with materialan aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate
7. concentrationconcentrated

ORD record

ord-28500ed702154fb2bcff98646342596c

Source dataset

uspto-grants-2012_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08318776B2