Triethyloxonium tetrafluoroborate → 1-ethoxy-2-(2,6-difluorophenyl)-1-(N-methylimino)-ethane

5.55 g (30 mmol) of 2,6-difluorophenylacetic acid methylamide are dissolved in 70 ml of dichloromethane, 7.4 g (39 mmol) of triethyloxonium tetrafluoroborate are added thereto and the whole is stirred for 25 hours at room temperature. The reaction mixture is then extracted by shaking in succession with cold 2N sodium carbonate solution, ice-water and cold saturated sodium chloride solution, dried over magnesium sulphate and concentrated. A mixture of ether and hexane is added to the residue, the unreacted educt remaining undissolved and being filtered off. The filtrate is concentrated and subjected to distillation in a bulb tube. 4 g (62.6% of the theoretical yield) of 1-ethoxy-2-(2,6-difluorophenyl)-1-(N-methylimino)-ethane which boils at 70° (0.02 mm) are obtained.

1. extractionThe reaction mixture is then extracted
2. stirringby shaking in succession with cold 2N sodium carbonate solution, ice-water and cold saturated sodium chloride solution
3. dry with materialdried over magnesium sulphate
4. concentrationconcentrated
5. additionA mixture of ether and hexane
6. additionis added to the residue
7. filtrationbeing filtered off
8. concentrationThe filtrate is concentrated
9. distillationsubjected to distillation in a bulb tube

ORD record

ord-a9d73528f0974c99b0daa21dc23db04a

Source dataset

uspto-grants-1991_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05045556