Methylamine → HCID 11391445、化合物
反応式
[CH3:1][NH2:2].IC[CH2:5][CH2:6][CH:7]([S:17][CH:18](CCCI)[CH2:19][CH2:20][C:21]([F:27])([F:26])[C:22]([F:25])([F:24])[F:23])CCC(F)(F)C(F)(F)F>O1CCCC1>[CH3:1][NH:2][CH2:5][CH2:6][CH2:7][S:17][CH2:18][CH2:19][CH2:20][C:21]([F:27])([F:26])[C:22]([F:25])([F:24])[F:23]参加物
4
反応条件
- 温度
- -60 °C
実験手順
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.