反应详情

温度

102 °C

21.6 g (131 mmol) 3-(3-pyridyl)-propionic acid methyl ester, 35.1 g ml (109 mmol) 4-(1-diphenylmethylpiperidine-4-yl)-butylamine and 9.8 g (54.5 mmol) 30% sodium methylate solution in methanol are heated to boiling in 480 ml toluene for five hours. Subsequently, 30 ml of solvent are distilled; thereby, sodium methylate precipitates and the temperature of the suspension increases to 102° C. under heavy foaming. The mixture is cooled to 70-80° C. and extracted twice with 45 ml and 30 ml of water. The organic phase is azeotropically dried on a moisture separator and cooled to ca. 0° C. The resulting precipitate is filtered off and crystallized from 190 ml toluol. Colorless crystals with a MP of 139° C. were recovered; yield: 46.3 g (93%).

1. distillationSubsequently, 30 ml of solvent are distilled
2. customthereby, sodium methylate precipitates
3. temperatureThe mixture is cooled to 70-80° C.
4. extractionextracted twice with 45 ml and 30 ml of water
5. customThe organic phase is azeotropically dried on a moisture separator
6. temperaturecooled to ca. 0° C
7. filtrationThe resulting precipitate is filtered off
8. customcrystallized from 190 ml toluol
9. customColorless crystals with a MP of 139° C. were recovered