1,1-Dichloroethane → Chloromethyl 4-trifluoromethylbenzoate

To 10 ml of dichloroethane were added 1 g of zirconium tetrachloride and 1 g of 4-trifluoromethylbenzoyl chloride, and the mixture was stirred at room temperature for 30 minutes. The mixture was cooled to 10° C., 0.16 g of trioxane was added, and the mixture was stirred for 30 minutes, and further stirred at room temperature for 1 hour. The mixture was cooled to 0° C., water was added slowly, 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 0.92 g of chloromethyl 4-trifluoromethylbenzoate.

1. temperatureThe mixture was cooled to 10° C.
2. stirringthe mixture was stirred for 30 minutes
3. stirringfurther stirred at room temperature for 1 hour
4. temperatureThe mixture was cooled to 0° C.
5. extractionthe resultant solution was extracted with chloroform three times
6. washwashed with an aqueous saturated sodium bicarbonate solution
7. dry with materialan aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate
8. concentrationconcentrated

ORDレコード

ord-78430b8516be4d819f31ab9e83827f65

出典データセット

uspto-grants-2012_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08318776B2