Hydrochloric Acid → HCID 178510584, compound

Temperature

50 °C

To 19.92 g of a toluene solution of 3,6-difluoropyrazine-2-carbonitrile with a concentration of 12.7% were sequentially added 18 ml of dimethyl sulfoxide, 9 ml of water, and 2.95 g of sodium acetate. The resulting mixture was heated to 50° C., and stirred at 50° C. for 7 hours. The mixture was then cooled to room temperature, and 9 ml of water and concentrated hydrochloric acid were added to adjust the pH to 2.5. 54 ml of ethyl acetate was added and a separation was performed. The separated organic layer was washed with 18 ml of water, and then washed with a 10% saline solution. Each of the aqueous layers was extracted with 18 ml of ethyl acetate, and the thus obtained organic layers were combined with the original organic layer. The ethyl acetate was then removed by distillation under reduced pressure, yielding 3.45 g of an oily 6-fluoro-3-hydroxypyrazine-2-carbonitrile.

1. temperatureThe mixture was then cooled to room temperature
2. customa separation
3. washThe separated organic layer was washed with 18 ml of water
4. washwashed with a 10% saline solution
5. extractionEach of the aqueous layers was extracted with 18 ml of ethyl acetate
6. customThe ethyl acetate was then removed by distillation under reduced pressure

ORD record

ord-6cb81d196bb448979599c087b8e612b6

Source dataset

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08835636B2