1,1-Dichloroethane → Chloromethyl 4-fluorobenzoate

To 10 ml of dichloroethane were added 1.32 g of zirconium tetrachloride and 1 g of 4-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 0.89 g of chloromethyl 4-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レコード

ord-87369aaad6e0408cb6b3e95f6feb0919

出典データセット

uspto-grants-2012_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08318776B2