Chloral Hydrate → HCID 87327711, compound

Participants

Reaction Steps

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+).

Provenance & Evidence