Methylamine → HCID 11391445, compound

45 g of methylamine are condensed at a bath temperature of −78° C. into a solution of 30.6 g of 3-iodopropyl-4,4,5,5,5-pentafluoropentyl sulphide in 200 ml of abs. tetrahydrofuran and the mixture is stirred at room temperature for 1.5 hours and at 60° C. for 4 hours in a pressure reactor. To open the reactor, it is allowed to cool overnight to room temperature and then to −78° C. It is then allowed to come to room temperature, excess methylamine is evaporated, the mixture is diluted with ethyl acetate, washed until neutral, dried over sodium sulphate and concentrated in vacuo, and the residue is chromatographed on silica gel using dichloromethane/methanol. 15.7 g of N-methyl-[3-(4,4,5,5,5-pentafluoro-pentylthio)propyl]amine are obtained as an oil.

1. temperatureto cool overnight to room temperature
2. customto −78° C
3. customto come to room temperature
4. customexcess methylamine is evaporated
5. additionthe mixture is diluted with ethyl acetate
6. washwashed until neutral,
7. dry with materialdried over sodium sulphate
8. concentrationconcentrated in vacuo
9. customthe residue is chromatographed on silica gel

ORD record

ord-3b7e9b58bee244ae8ebaf4ae893669c7

Source dataset

uspto-grants-2004_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06677324B1