Water → HCID 54064235, Verbindung

4.32 g (0.02 mol) of 3-phenoxy-4-fluoro-benzaldehyde and 6.96 g (0.02 mol) of 2,2-dimethyl-3-(2-bromo-2-(4-chlorophenyl)-vinyl)-cyclopropanecarboxylic acid chloride were together added dropwise to a mixture of 1.6 g of sodium cyanide, 2.5 ml of water, 100 ml of n-hexane and 0.5 g of tetrabutylammonium bromide at 20°-25° C., while stirring, and the mixture was then stirred at 20°-25° C. for 4 hours. 300 ml of toluene were then added to the reaction mixture and the mixture was extracted by shaking twice with 300 ml of water each time. The organic phase was separated off and dried over magnesium sulphate and the solvent was distilled off under a waterpump vacuum. Last residues of solvent were removed by brief incipient distillation at a bath temperature of 60° C./1 mm Hg. 7.8 g (70.3% of theory) of 2,2-dimethyl-3-(2-bromo-2-(4-chloro-phenyl)-vinyl)-cyclopropanecarboxylic acid 3-phenoxy-4-fluoro-α-cyano-benzyl ester were obtained as a viscous oil. The structure was confirmed by the 1H-NMR spectrum.

1. stirringthe mixture was then stirred at 20°-25° C. for 4 hours
2. extractionthe mixture was extracted
3. stirringby shaking twice with 300 ml of water each time
4. customThe organic phase was separated off
5. dry with materialdried over magnesium sulphate
6. distillationthe solvent was distilled off under a waterpump vacuum
7. customLast residues of solvent were removed by brief incipient distillation at a bath temperature of 60° C./1 mm Hg

ORD-Eintrag

ord-55975649e6a3405fb7c963e980b7757d

Quelldatensatz

uspto-grants-1981_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04279920