Water → 3,5-Dichlorobenzyl chloride

Under a nitrogen atmosphere, a stirred solution of 25.0 grams (0.141 mole) of 3,5-dichlorophenylmethanol and 11.4 mL (0.141 mole) of pyridine in 200 mL of chloroform was cooled to 5° C., and 15.9 mL (0.218 mole) of thionyl chloride was added dropwise during a 10 minute period. Upon completion of addition, the reaction mixture was allowed to warm to ambient temperature where it was stirred for about 18 hours. After this time, the reaction mixture was poured into 300 mL of water, and the mixture was extracted with 600 mL of diethyl ether. The ether solution was washed with 70 mL of an aqueous 6N hydrochloric acid solution, and then it was concentrated under reduced pressure to a residual oil. The oil was distilled under reduced pressure, yielding 25.6 grams of 3,5-dichlorophenylmethyl chloride, bp 95°-100° C./0.1 mm Hg.

1. additionUpon completion of addition
2. extractionthe mixture was extracted with 600 mL of diethyl ether
3. washThe ether solution was washed with 70 mL of an aqueous 6N hydrochloric acid solution
4. concentrationit was concentrated under reduced pressure to a residual oil
5. distillationThe oil was distilled under reduced pressure

ORD 기록

ord-5dab5f99bd144a6aa0afc6f6b64993af

출처 데이터셋

uspto-grants-1996_07

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US05536725