2-Methylpyridine → HCID 13185026, compound

Participants

Reaction Steps

In a 50 ml 3-neck RBF equipped with a magnetic stir bar, thermocouple probe, addition funnel, nitrogen inlet adapter, and a rubber septum, charged dichloromethane (anh) (2.5 ml) and 2-picoline (1.46 ml, 14.7 mmol). This 2-picoline solution was chilled in an ice/NaCl bath to −2° C. Then a solution of chlorosulfonic acid (0.478 ml, 7.14 mmol) in dichloromethane (anh) (2.5 ml) was added over 30 minutes, with the temperature being maintained below 5° C. The resulting orange solution was stirred for 30 minutes before being added to the sulfation reaction at room temperature as described in this Example, step 2.

Provenance & Evidence