Methylamine → HCID 11391445, compound

Temperature

60 °C

In a solution of 30.6 g of 3-iodopropyl-4,4,5,5,5-pentafluoropentylsulfide in 200 ml of absolute tetrahydrofuran, 45 g of methylamine is condensed at a bath temperature of ±78° C., and it is stirred for 1.5 hours at room temperature and for 4 hours at 60° C. in the 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 reach room temperature, excess methylamine is evaporated, 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-pentafluoropentylthio)-propyl]-amine is obtained as an oil.

1. customcondensed at a bath temperature of ±78° C., and it
2. temperatureto cool overnight to room temperature
3. customto −78° C
4. customto reach room temperature
5. customexcess methylamine is evaporated
6. additiondiluted with ethyl acetate
7. washwashed neutral
8. customdried on sodium sulfate
9. concentrationconcentrated by evaporation in a vacuum
10. customchromatographed on silica gel with dichloromethane/methanol

ORD record

ord-cd3db5db45024e6a9c155402257142b3

Source dataset

uspto-grants-2001_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06271403B1