Chloral Hydrate → HCID 87408991, compound

Temperature

80 °C

To a solution of sodium sulphate (8.69 g, 61.15 mmol) in water (20 ml) was added chloralhydrate (0.62 g, 3.74 mmol) at ambient temperature. To the resulting clear solution was added a solution of 5-methyl-6-aminoindazol (0.5 g, 3.4 mmol, prepared as described in Eur. Pat. Appl. EP 040872) in 1N aqueous hydrochloric acid (3.7 ml). The resulting mixture turned cloudy and hydroxylamine hydrochloride (0.75 g, 10.9 mmol) was then added. The resulting reaction mixture was heated-up gradually from ambient temperature to 80° C. When the reaction mixture has reached an internal temperature of 80° C., it was stirred for an additional 30 min at 80° C. The reaction mixture was then cooled down to ambient temperature with an ice bath. The reaction mixture was filtrated. The filtercake was washed thoroughly with water and dried at 50° C. for 15 hours to afford the desired product as a brown powder of >95% purity according to HPLC. LC/MS: 219 (M+H)+.

1. customThe resulting reaction mixture
2. temperaturewas heated-up gradually from ambient temperature to 80° C
3. customan internal temperature of 80° C., it
4. temperatureThe reaction mixture was then cooled down to ambient temperature with an ice bath
5. filtrationThe reaction mixture was filtrated
6. washThe filtercake was washed thoroughly with water
7. customdried at 50° C. for 15 hours

ORD record

ord-9198c3e02129428f91b259bb02dd4f6e

Source dataset

uspto-grants-2013_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08598078B2