Hydrochloric Acid → 2-Bromo-4,6-bis(trifluoromethyl)benzaldehyde

Temperatur

-78 °C

A 2.59 M hexanes solution of n-BuLi (1.13 mL, 2.92 mmol) was added dropwise to a, 0° C., THF solution (4 mL) of 2,2,6,6-tetramethylpiperidine (0.50 mL, 2.92 mmol). After 5 min at 0° C., the solution was cooled to −78° C. and 1-bromo-3,5-bis(trifluoromethyl)benzene was added dropwise over 2 min. The resulting brown amber colored solution was stirred at −78° C. for an additional 20 min. Ethyl formate (0.587 mL, 7.30 mmol) was then added dropwise at −78° C. over 1 min. After 30 min at −78° C., 1 M aqueous HCl was added, the layers were separated and the organic layer was washed with 0.1 M aqueous HCl and 1 M aqueous. The organic layer was dried (Na2SO4), concentrated, and short path vacuum distilled to provide the title compound.

1. waitAfter 30 min at −78° C.
2. customthe layers were separated
3. washthe organic layer was washed with 0.1 M aqueous HCl and 1 M aqueous
4. dry with materialThe organic layer was dried (Na2SO4)
5. concentrationconcentrated
6. distillationshort path vacuum distilled

ORD-Eintrag

ord-9e6e1e238479481e94e033818886ccae

Quelldatensatz

uspto-grants-2014_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08748624B2