Sulfuric Acid → Pyridine-2-sulfonyl Chloride

Temperature

-5 °C

2-Mercaptopyridine (available from Sigma-Aldrich; 0.25 g, 2.25 mmol) was added to H2SO4 (8 mL) and the mixture was cooled to about −5° C. Sodium hypochlorite (10% solution; 17 mL) was added and the reaction mixture was stirred for 30 min at about 0° C. Water (10 mL) was added and the mixture was extracted with CH2Cl2 (3×20 mL). The combined organic layers were dried over Na2SO4, filtered and evaporated under reduced pressure to give crude pyridine-2-sulfonyl chloride (0.23 g, 58%), which was used directly in the next step without further purification.

1. extractionthe mixture was extracted with CH2Cl2 (3×20 mL)
2. dry with materialThe combined organic layers were dried over Na2SO4
3. filtrationfiltered
4. customevaporated under reduced pressure

ORD record

ord-cf77b026dd444521b1f03dfd056c4460

Source dataset

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08691993B2