反应详情

温度

62.5 °C

13.8 g (30 mmol) of 2-(5-fluoro-2-{[4′-(trifluoromethyl)biphenyl-4-yl]methoxy}phenyl)ethylamine hydrochloride [obtainable by taking up the compound of Example 45A in a 1 M solution of hydrogen chloride in dioxane, reconcentrating the solution and drying the resulting residue] are introduced into 200 ml of DMF, mixed with 32.4 ml (0.23 mol) of triethylamine and heated to 60-65° C. At this temperature, 9.48 g (0.05 mol) of ethyl 5-bromovalerate are added dropwise, and the mixture is stirred for 12 hours. After cooling, the mixture is added to water, adjusted to pH 5 with 1 M hydrochloric acid and extracted with ethyl acetate. The organic phase is dried over sodium sulfate and the solvent is removed in vacuo. The resulting residue is purified by chromatography on silica gel (mobile phase: dichloromethane/methanol 10:1). 4.5 g (8.9 mmol, 18% of theory) of the title compound are obtained.

1. customdrying the resulting residue]
2. additionare introduced into 200 ml of DMF
3. temperatureAfter cooling
4. extractionextracted with ethyl acetate
5. dry with materialThe organic phase is dried over sodium sulfate
6. customthe solvent is removed in vacuo
7. customThe resulting residue is purified by chromatography on silica gel (mobile phase: dichloromethane/methanol 10:1)