Chloral Hydrate → HCID 87441566, compound

Participants

Reaction Conditions

Reaction Steps

Sodium sulfate (20.75 g, 146 mmol) and chloral hydrate (2.78 g, 17 mmol) were dissolved in water (30 mL). Then a solution of 2,4-di-tert-butyl-phenylamine [prepared according to P. D. Bartlett, M. Roha, R. M. Stiles, J. Am. Chem. Soc. 1954, 76, 2349-2353](3 g, 14.6 mmol) in water (6 mL), 25% HCl (1.9 mL), and a solution of hydroxylamine hydrochloride (3.25 g, 47 mmol) in water (8 mL) were added. The mixture was heated at 100° C. for 1 h. Extraction with ethyl acetate and chromatography on silica gel with a gradient of 0% to 25% of ethyl acetate in heptane afforded a light brown solid (1 g, 25%), which was a 1:1-mixture with formulated starting material. MS: m/z=277 (M+H).

Provenance & Evidence