Methylamine → HCID 11391445, compound

Participants

Reaction Conditions

Reaction Steps

45 g of methylamine is condensed in a solution of 30.6 g of 3-iodopropyl-4,4,5,5,5-pentafluoro-pentylsulfide in 200 ml of absolute tetrahydrofuran at a bath temperature of −78° C., and it is stirred for 1.5 hours at room temperature as well as for 4 hours at 60° C. in a pressurized reactor. To open the reactor, it is allowed to cool overnight to room temperature and then to −78° C. Then, it is allowed to come to room temperature, excess methylamine is evaporated, it is diluted with ethyl acetate, washed neutral, dried on sodium sulfate, concentrated by evaporation in a vacuum and chromatographed on silica gel with dichloromethane/methanol. 15.7 g of N-methyl-[3-(4,4,5,5,5-pentafluoro-pentylthio)-propyl]-amine is obtained as an oil.

Provenance & Evidence