Methylamine → HCID 11391445, compound

Temperature

-60 °C

45 g of methylamine is condensed in a solution of 30.6 g of 3-iodopropyl-4,4,5,5,5-pentafluoropentyl sulfide in 200 ml of absolute tetrahydrofuran 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 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 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 methyl-[3-(4,4,5,5,5-pentafluoropentylthio)-propyl]-amine is obtained as an oil.

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

ORD record

ord-17d437c1884d491c8431dd808ecb2b8e

Source dataset

uspto-grants-2001_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06288051B1