反应详情

温度

2 °C

(S)-3-(dimethylamino)-2-methyl-1-(3-nitro-phenyl)-propan-1-one (100 g, 0.423 mol), methyl-tetrahydrofuran (400 ml) and Pd/C 5%, anhydrous (4.0 g) are added into a 1 liter autoclave, at room temperature. The suspension is cooled to 0-4° C., then it is hydrogenated at 2 bars of hydrogen gas without exceeding 8° C. The conversion is monitored using HPLC and it is deemed complete when the HPLC area % of the initial product and the reaction intermediates is <0.3. Then catalyst is filtered and the solution can be used as it is in the subsequent step or concentrated under vacuum at 45-50° C. to oily residue. About 86 g of yellow to dark red oil are obtained (about 98% yield, ee≧97%, purity ≧92%).

1. customwithout exceeding 8° C
2. filtrationThen catalyst is filtered
3. concentrationconcentrated under vacuum at 45-50° C. to oily residue
4. customAbout 86 g of yellow to dark red oil are obtained (about 98% yield, ee≧97%, purity ≧92%)