Methylamine → 1,1,1-trifluoro-N-methyl-methanesulfonamide

A weighed pressure reactor (available from Parr Instrument Co., Moline, Ill.) is charged with dichloromethane (100 mL) and is then cooled using liquid nitrogen. Methylamine is introduced from a cylinder via a stainless steel tube that is connected to a valve on the reactor. The reactor is periodically weighed, and methylamine is added until 20 g have been added. Trifluoromethanesulfonylfluoride is then introduced into the reactor from a cylinder via a stainless steel tube until 97.9 g have been added. The pressure reactor is then sealed and is placed in a motorized rocker and is rocked and allowed to warm to room temperature. After a period of about 6 hours after the reactor reaches room temperature, it is slowly vented to the atmosphere by opening the valve. The product residue is washed with 10 weight percent aqueous HCl and the organic phase is then dried over MgSO4. The mixture is filtered and the solvent is removed from the filtrate using a rotary evaporator to afford the product.

1. temperatureis then cooled
2. customis connected to a valve on the reactor
3. additionhave been added
4. additionhave been added
5. customThe pressure reactor is then sealed
6. washThe product residue is washed with 10 weight percent aqueous HCl
7. dry with materialthe organic phase is then dried over MgSO4
8. filtrationThe mixture is filtered
9. customthe solvent is removed from the filtrate
10. customa rotary evaporator
11. customto afford the product

ORD record

ord-db49350b58e742288361901614184dff

Source dataset

uspto-grants-2010_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07675058B2