反应详情

温度

5 °C

A 100 l double wall jacketed reaction vessel with electric impeller stirrer, gas transfer line, Pt100 temperature sensor and oil-based cooling and heating system was charged with the 10 kg (39.8 mol) of the mixture of (2R,3R)-1-dimethylamino-3-(3-methoxyphenyl)-2-methylpentan-3-ol (97%) and (2S,3S)-1-dimethylamino-3-(3-methoxyphenyl)-2-methylpentan-3-ol (3%) from step b) in 45 l of acetone at 20° C. and a stirrer speed of 100 rpm. The solution was cooled to 5° C. Within 20 min, approx. 1.3 kg of gaseous hydrogen chloride were passed over the solution, the temperature in the vessel rising continuously to 28° C. despite cooling. The hydrogen chloride was taken from a hydrogen chloride cylinder which was connected to the gas transfer line of the vessel through a pressure reduction valve and hose and was placed on a balance for weight measurement. Further gaseous hydrogen chloride was then passed over until a 5 ml sample of the solution diluted with 10 ml of water had a pH value of 1-3. The solution was stirred at 5° C. for 2 h. The suspension was centrifuged off in a centrifuge and washed once with 7 l of acetone. The product was dried in a drying cabinet at 40° C. for 24 h under reduced pressure to a final pressure of 20 mbar. 9.73 kg (85% of theoretical) of colourless (2R,3R)-1-dimethylamino-3-(3-methoxyphenyl)-2-methylpentan-3-ol hydrochloride with an enantiomeric purity of 100% were obtained.

1. temperatureheating system
2. customrising continuously to 28° C.
3. temperaturedespite cooling
4. customwas connected to the gas transfer line of the vessel through a pressure reduction valve
5. washwashed once with 7 l of acetone
6. customThe product was dried in a drying cabinet at 40° C. for 24 h under reduced pressure to a final pressure of 20 mbar