2-Methylpyridine → HCID 13185026, compound

Temperature

-6.199999809265137 °C

To a 50 ml 3-neck RBF equipped with a magnetic stir bar, thermocouple probe, addition funnel, nitrogen inlet adapter, and a rubber septum, was charged anhydrous dichloromethane (Volume: 7.5 ml) and 2-picoline (4.38 ml, 44.2 mmol). The mixture was chilled in an ice/NaCl bath to −6.2° C. A solution of chlorosulfonic acid (1.434 ml, 21.41 mmol) in anhydrous dichloromethane (Volume: 7.5 ml) was added over 30 minutes, with the temperature being maintained below 5° C., to give an orange solution. The solution was stirred for 30 minutes, split solution into 2 equal parts (9.5 ml each). One part was added to the sulfation reaction at room temperature as described in this Example, step 2.

1. customTo a 50 ml 3-neck RBF equipped with a magnetic stir bar
2. additionthermocouple probe, addition funnel, nitrogen inlet adapter
3. temperaturebeing maintained below 5° C.
4. customto give an orange solution
5. customsplit solution into 2 equal parts (9.5 ml each)
6. additionOne part was added to the sulfation reaction at room temperature

ORD record

ord-32e7fc16666144c48feed12b8de7888f

Source dataset

uspto-grants-2015_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09120796B2