反应详情

温度

50 °C

The mixture is cooled to 50° C. and 15.5 g (0.0572 mol) crude N-(trans-3-chloro-2-propenyl)-N-methyl-1-naphthalene-methylamine, 20 ml THF and 74 mg NiCl2 (0.77 molar percent) introduced. The reaction mixture is heated at 90°-95° C. for 1 hour, cooled to 20°/25° C. and 130 ml of a 2.5% (w/v) aqueous solution of EDTA disodium salt added, the phases are separated and the aqueous phase re-extracted with 70 ml chilled toluene. The combined organic phases are washed with 2×90 ml water and concentrated to a residue, thus giving 18.2 g (greater than theoretical yield) terbinafine with a purity of 83.6% (HPLC A %).

1. temperatureThe reaction mixture is heated at 90°-95° C. for 1 hour
2. additionadded
3. customthe phases are separated
4. extractionthe aqueous phase re-extracted with 70 ml
5. temperaturechilled toluene
6. washThe combined organic phases are washed with 2×90 ml water
7. concentrationconcentrated to a residue