反应详情

温度

50 °C

To a stirring solution of (2-chloro-3-trifluoromethyl-benzyl)-(2,2-diphenyl-ethyl)-[3-(3-piperazin-1-yl-phenoxy)-propyl]-amine (150 mg, 2.46 mmol) in anhydrous DMF (20 ml) was added iodomethane (16.8 uL, 2.71 mmol) and diisopropylethylamine (86 uL, 4.93 mmol). The resulting solution was heated at 50° C. for 4 hours and then concentrated. Purification by flash silica gel chromatography (silica gel 60, EM science; 3% MeOH and 0.5% NH2OH in CH2Cl2) afforded the N-methylated product. The amine was dissolved in CH2Cl2 and methansulfonic acid (2 equivalents) was added. The methylene chloride solution was concentrated and the resulting bis-methanesulfonate salt was dried under vacuum to yield the title compound as a solid, 56 mg (37%). MS(ES) m/e 622.4 (M+).

1. concentrationconcentrated
2. customPurification by flash silica gel chromatography (silica gel 60, EM science; 3% MeOH and 0.5% NH2OH in CH2Cl2)
3. customafforded the N-methylated product
4. concentrationThe methylene chloride solution was concentrated
5. dry with materialthe resulting bis-methanesulfonate salt was dried under vacuum