1,1-Dichloroethane → HCID 12347626, compound

To 10 ml of dichloroethane were added 1 g of zirconium tetrachloride and 1 g of 3-trifluoromethylbenzoyl chloride, and the mixture was stirred at room temperature for 30 minutes. At 10° C., 0.16 g of trioxane was added, and the mixture was stirred for 30 minutes, and further stirred at room temperature for 2 hours. 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. The residue was subjected to silica gel column chromatography to obtain 0.4 g of chloromethyl 3-trifluoromethylbenzoate.

1. stirringthe mixture was stirred for 30 minutes
2. stirringfurther stirred at room temperature for 2 hours
3. temperatureThe mixture was cooled to 0° C.
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-5c7a0197c4d443e592c6626aa9e8dd11

Source dataset

uspto-grants-2012_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08318776B2