2-Methylpyridine → HCID 13185026, compound

Participants

Reaction Steps

To a 100 ml 3-neck RBF equipped with a magnetic stir bar, thermocouple probe, addition funnel, nitrogen inlet adapter, and a rubber septum, was charged dichloromethane (anh) (25 ml) and 2-picoline (11.88 ml, 120 mmol). This picoline solution was chilled in an ice/NaCl bath to −3.5° C. Then a solution of chlorosulfonic acid (3.82 ml, 57.1 mmol) in dichloromethane (anh) (25 ml) was added over 50 minutes, with the temperature being maintained below 5° C. The resulting pale yellow solution was stirred for 1 h at room temperature before being added to the sulfation reaction at room temperature as described in this Example, step 2.

Provenance & Evidence