18-Crown-6 → HCID 14692897、化合物

Into a three-necked 50 ml flask equipped with a condenser and a stirrer, 1.9 g (33 mmol) of spray-dried potassium fluoride (purchased from Laporte Industry), 1.1 g (2.5 mmol) of tetraphenyl phosphonium bromide, 0.7 g (2.5 mmol) of 18-crown-6 and 6.4 g (25 mmol) of ethyl 3,4,5-trichlorobenzoate were introduced, and the mixture was heated in an oil bath and reacted under a nitrogen atmosphere at 210° C. for 2 hours. The reactor was cooled, and the mixture was diluted with 40 ml of toluene. Inorganic salts were filtered off, and toluene was concentrated to give the residue, which was distilled under reduced pressure to obtain 3.4 g of ethyl 3,5-dichloro-4-fluorobenzoate. The yield was 57%. The physical properties are shown below.

1. customInto a three-necked 50 ml flask equipped with a condenser and a stirrer
2. temperaturethe mixture was heated in an oil bath
3. customreacted under a nitrogen atmosphere at 210° C. for 2 hours
4. temperatureThe reactor was cooled
5. filtrationInorganic salts were filtered off
6. concentrationtoluene was concentrated
7. customto give the residue, which
8. distillationwas distilled under reduced pressure

ORDレコード

ord-59e92231a82e4f48ba00919ea02ca637

出典データセット

uspto-grants-1990_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04916253