反应详情

温度

60 °C

(R)-3-(1-(naphthalen-1-yl)ethylamino)-1-(3-(trifluoromethyl)phenyl)propan-1-ol hydrochloride (IXa) (20.0 g, 48.796 mmol) is suspended in toluene (140 ml) at 40° C. and phosphoryl chloride (4.3 g, 28.044 mmol) is added drop-wise over 10 minutes. The reaction mixture is stirred two hours at 60° C., then DMF (1.0 g) is added at 40° C., followed by additional phosphoryl chloride (3.2 g, 20.870 mmol). The mixture is stirred at 40° C. overnight and then MTBE (40 ml) is added. Volatiles are removed by repeatedly distilling off under vacuum and restoring MTBE. After that a 1:1 vol/vol toluene/MTBE solution is received, which is heated up to 70° C. and allowed to cool down slowly to 15°-20° C. the so-obtained precipitate is aged at room temperature overnight, then filtered and washed with a 1:1 vol/vol toluene/MTBE mixture (3×12 ml). (R)-3-chloro-N-(1-(naphthalen-1-yl)ethyl)-3-(3-(trifluoromethyl)phenyl)propan-1-amine hydrochloride (X) is obtained as a white powder after exsiccation at 55° C. under vacuum (6.0 g, 14.008 mmol, yield: 28.7%).

1. stirringThe mixture is stirred at 40° C. overnight
2. customVolatiles are removed
3. distillationby repeatedly distilling off under vacuum
4. temperaturewhich is heated up to 70° C.
5. temperatureto cool down slowly to 15°-20° C. the so-obtained precipitate
6. waitis aged at room temperature overnight
7. filtrationfiltered
8. washwashed with a 1:1 vol/vol toluene/MTBE mixture (3×12 ml)