反应详情

To an Agilent HPLC system fitted with a diode array detector and a 0.46 cm ID×25 cm long 10 mm KROMASIL Silica Column was charged 714 mg of racemic R-(+)-1-phenyl-ethyl)-carbamic acid-2,6-di-sec-butylphenyl ester dissolved in 10 ml of hexane/ethyl acetate (98:2) to give a 71.4 g/l feed solution. The sample was eluted with hexane/ethyl acetate (98:2) at 2 ml/min at 25° C. Fractions containing (R,R,R)-1-phenylethylcarbamic acid-2,6-di-sec-butylphenyl ester were collected and evaporated under reduced pressure at <55° C. At the highest loading, the (R,R,R)-stereoisomer was collected with a chiral purity of 98.7% diastereomeric excess (de) and a total yield of 53%.

1. customTo an Agilent HPLC system fitted with a diode array detector
2. customto give a 71.4 g/l feed solution
3. washThe sample was eluted with hexane/ethyl acetate (98:2) at 2 ml/min at 25° C
4. additionFractions containing (R,R,R)-1-phenylethylcarbamic acid-2,6-di-sec-butylphenyl ester
5. customwere collected
6. customevaporated under reduced pressure at <55° C
7. customAt the highest loading, the (R,R,R)-stereoisomer was collected with a chiral purity of 98.7% diastereomeric excess (de)