Pyridine → HCID 18792316, Verbindung

Then, 1.2 g (6.1 mmol) of 3,5-difluoro-4-trifluoromethyl-phenol, 0.7 ml of pyridine, and 2 ml of toluene were mixed. To this mixture was added dropwise 3 ml of toluene solution containing 6.1 mmol 2-fluoro-4-propylbenzoyl chloride at room temperature in 10 minutes. After the dropping was finished, they were reacted at 50° C. for 2 hours. After finishing of the reaction, 10 ml of water was added to the reaction product and then extracted with 30 ml of toluene. The organic layer thus obtained was washed with 6N-hydrochloric acid thrice, 2N-sodium hydroxide thrice, and water thrice, and then dried over anhydrous magnesium sulfate. Solvent was distilled off at a reduced pressure and the residue was subjected to a silica gel column chromatography (eluent: toluene) to obtain 2.0 g of a crude 3,5-difluoro-4-trifluormethylphenyl 2-fluoro-4-propylbenzoate. This product was recrystallized from a mixed solvent of heptane/ether (1/1) to obtain 1.1 g (yield: 50.2%) of the subject compound.

1. customthey were reacted at 50° C. for 2 hours
2. additionwas added to the reaction product
3. extractionextracted with 30 ml of toluene
4. customThe organic layer thus obtained
5. washwas washed with 6N-hydrochloric acid thrice, 2N-sodium hydroxide thrice, and water thrice
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationSolvent was distilled off at a reduced pressure

ORD-Eintrag

ord-0c2f603a24354b049731c2223765eb4d

Quelldatensatz

uspto-grants-2000_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06051288