Hydrochloric Acid → HCID 178494844, compound

Temperature

85 °C

Into a 50-mL round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed a solution of 3-(2-methoxyethyl)-N,N,4-trimethyl-1H-pyrazole-1-sulfonamide (compound 305.3, 440 mg, 1.78 mmol) in dioxane (10 mL). HCl (10 mL, 6 M, 30 mmol) was added to the reaction mixture. The reaction mixture was stirred for 1 h at 85° C., then cooled to room temperature and carefully neutralized with NaHCO3 aq (sat.) to pH=8. The aqueous phase was extracted with 3×50 mL of EtOAc and the combined organic layers were dried over Na2SO4. After filtration, the filtrate was concentrated under reduced pressure to give the crude product which was used in the next step without further purification.

1. customInto a 50-mL round-bottom flask purged
2. temperaturemaintained with an inert atmosphere of nitrogen
3. temperaturecooled to room temperature
4. extractionThe aqueous phase was extracted with 3×50 mL of EtOAc
5. dry with materialthe combined organic layers were dried over Na2SO4
6. filtrationAfter filtration
7. concentrationthe filtrate was concentrated under reduced pressure

ORD record

ord-acc8a3cc04f340f6936ad103fcdf1051

Source dataset

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09428502B2