托莫西汀杂质13

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 1.15 g of trans-N-cinnamyl-methylamine in 20 ml of dimethylformamide are slowly added dropwise with stirring to 1.4 g of 4-chloromethyl-2H-1-benzopyrane and 0.8 g of sodium carbonate in 40 ml dimethylformamide. Stirring is continued for 24 hours at room temperature, the resulting mixture evaporated under vacuum and the residue taken up in ethylacetate/water. The organic phase is separated, washed with 1% tartaric acid, saturated NaHCO3 and saturated NaCl, dried over MgSO4 and concentrated by evaporation. After purification by chromatography on kieselgel (eluant toluene/ethylacetate 10/1) the title compound is obtained. the resulting mixture evaporated under vacuum The organic phase is separated washed with 1% tartaric acid, saturated NaHCO3 and saturated NaCl dried over MgSO4 concentrated by evaporation After purification by chromatography on kieselgel (eluant toluene/ethylacetate 10/1) the title compound is obtained

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 1.15 g of trans-N-cinnamyl-methylamine in 20 ml of dimethylformamide are slowly added dropwise with stirring to 1.4 g of 4-chloromethyl-2H-1-benzopyrane and 0.8 g of sodium carbonate in 40 ml dimethylformamide. Stirring is continued for 24 hours at room temperature, the resulting mixture evaporated under vacuum and the residue taken up in ethylacetate/water. The organic phase is separated, washed with 1% tartaric acid, saturated NaHCO3 and saturated NaCl, dried over MgSO4 and concentrated by evaporation. After purification by chromatography on kieselgel (eluant toluene/ethylacetate 10/1) the title compound is obtained. the resulting mixture evaporated under vacuum The organic phase is separated washed with 1% tartaric acid, saturated NaHCO3 and saturated NaCl dried over MgSO4 concentrated by evaporation After purification by chromatography on kieselgel (eluant toluene/ethylacetate 10/1) the title compound is obtained

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 1.15 g of trans-N-cinnamyl-methylamine in 20 ml of dimethylformamide are slowly added dropwise with stirring to 1.4 g of 4-chloromethyl-2H-1-benzopyrane and 0.8 g of sodium carbonate in 40 ml dimethylformamide. Stirring is continued for 24 hours at room temperature, the resulting mixture evaporated under vacuum and the residue taken up in ethylacetate/water. The organic phase is separated, washed with 1% tartaric acid, saturated NaHCO3 and saturated NaCl, dried over MgSO4 and concentrated by evaporation. After purification by chromatography on kieselgel (eluant toluene/ethylacetate 10/1) the title compound is obtained. the resulting mixture evaporated under vacuum The organic phase is separated washed with 1% tartaric acid, saturated NaHCO3 and saturated NaCl dried over MgSO4 concentrated by evaporation After purification by chromatography on kieselgel (eluant toluene/ethylacetate 10/1) the title compound is obtained