反应详情

(+-)3-dimethylamino-l-phenyl-1-propanol (10) (19 g) was dissolved in CH2Cl2 (200 ml). The solution was saturated with HCl (g). Thionyl chloride (17 ml) was added dropwise over 20 min. resulting in slight reflux. Subsequental reflux for 5 h resulted in the formation of a precipitate. Cooling and evaporation of the reaction mixture resulted in a yellowish crystalline mass, which was rinsed by several washings with acetone, resulting in colourless crystals of the title compound identified by 1H NMR.

1. customresulting in slight reflux
2. temperatureSubsequental reflux for 5 h
3. customresulted in the formation of a precipitate
4. temperatureCooling
5. customevaporation of the reaction mixture
6. customresulted in a yellowish crystalline mass, which
7. washwas rinsed by several washings with acetone