Ammonium Hydroxide → pyridine-3-sulfonamide

To a suspension of 3-pyridinesulfonyl chloride hydrochloride (5.00 g) in acetone (8.5 ml) was added ammonia aqueous solution (28%, 8.5 ml) at 0° C. dropwise and stirred at room temperature for 3 hours. The solution was evaporated and poured into water (ca. 10 ml), ethyl acetate (100 ml) and tetrahydrofuran (100 ml). The organic layer was washed with brine twice and the aqueous layer was extracted with ethyl acetate (90 ml) and methanol (10 ml). The combined organic layer was dried over magnesium sulfate, evaporated and crystallized in hexane and ethyl acetate to give 3-pyridinesulfonamide (3.45 g).

1. customThe solution was evaporated
2. additionpoured into water (ca. 10 ml), ethyl acetate (100 ml) and tetrahydrofuran (100 ml)
3. washThe organic layer was washed with brine twice
4. extractionthe aqueous layer was extracted with ethyl acetate (90 ml) and methanol (10 ml)
5. dry with materialThe combined organic layer was dried over magnesium sulfate
6. customevaporated
7. customcrystallized in hexane

ORD record

ord-aad9279762d34e7d9da71761f5b3e8d0

Source dataset

uspto-grants-2011_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07928264B2