Chloral Hydrate → HCID 87327711, Verbindung

A mixture of 3-bromo-5-fluoroaniline (4.0 g, 21.1 mmol, 1.0 equiv) in conc. HCl (10 mL) and water (100 mL) was heated until it became a clear solution. 2,2,2-trichloroethane-1,1-diol (3.83 g, 23.2 mmol, 1.1 equiv) and Na2SO4 (22.5 g, 158.5 mmol, 7.3 equiv.) was pre-warmed to 50° C. and added to the mixture. To the stirred mixture was then added an aqueous solution of hydroxylammonium chloride (4.39 g, 63.2 mmol, 3.0 equiv) dropwise. The resulting mixture was refluxed for 1 h. After it was cooled to room temperature, the precipitate was filtered and washed with excess water, dried under vacuum to provide 6.13 g of crude product, which was used into the next step without further purification. MS (ESI): 259, 261 (MH+).

1. temperaturewas heated until it
2. additionadded to the mixture
3. temperatureThe resulting mixture was refluxed for 1 h
4. filtrationthe precipitate was filtered
5. washwashed with excess water
6. customdried under vacuum

ORD-Eintrag

ord-e38aa9d880284845852574f43b91defb

Quelldatensatz

uspto-grants-2014_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08772301B2