反应详情

温度

57.5 °C

A 500 ml three-necked round-bottom flask, under nitrogen atmosphere, is added with raceme 3-(isopropoxycarbonyl-amino-methyl)-5-methyl-hexanoic acid (44.2 g, 0.180 moles), triethylamine (8.20 g, 0.081 moles) and (S)-(−)-phenyl-ethylamine (12.00 g; 0.099 moles) in a 95:5 water/isopropanol mixture (200 ml) heated at 55-60° C. The mixture is spontaneously left to cool to room temperature, then it is cooled to 0-5° C. for at least 1 h. The solid is filtered off and washed with cool water (2×20 ml) and then with cool toluene (4×20 ml), it is dried in oven at 55-60° C. for 16-18 h. 27.0 g of white solid are obtained with an enantiomer ratio of 99:1.

1. waitThe mixture is spontaneously left
2. temperatureto cool to room temperature
3. temperatureit is cooled to 0-5° C. for at least 1 h
4. filtrationThe solid is filtered off
5. washwashed with cool water (2×20 ml)
6. dry with materialwith cool toluene (4×20 ml), it is dried in oven at 55-60° C. for 16-18 h