with a DAD detector and a Phenomenex Cellulose-4 column (4.6 mm ×
250 mm, i.d. 5 μm, Phenomenex, CA). A pair of enantiomers (+)-
respectively, by employing MeOH–H2O (80:20, v/v)
as the mobile phase, with a flow rate of 1 mL/min.
Cellulose-4 is a high-performance liquid chromatography (HPLC) stationary phase manufactured by Phenomenex. It is designed for the separation and analysis of polar compounds. The phase consists of a chemically bonded cellulose-based sorbent material.
Example 124
The R and S enantiomers of racemic compounds and the diastereomers (including cis- and trans-) of compounds were separated using either Chiral SFC or Chiral HPLC or preparative HPLC or SFC utilizing different columns such as XBridge Shield RP18 OBD, (CHIRALCEL OJ, CHIRALCEL OD, ChiralPAK AD, (R,R)-WHELK-O1-Kromasil, ChiralPAK IA, ChiralPAK IC, ChiralPAK ID, Lux Cellulose-4, SHIMADZU-SPD-20A, Phenomenex Lux, Cellulose-4, Amchemteq ACl Am-1 with different dimensions and diameter.
Columns were eluted with two mobile phases (Phase A and Phase B) with gradient from 0 to 100% for both phases. Some examples of phases used but not limited: 0.1% diethylamine in MeOH, water (0.05% TFA), MeCN, Hexane (0.1% diethylamine or diisopropylamine), MeOH, dichloromethane, isopropanol, ethanol, MTBE, 0.2% isopropanol in EtOH, 0.1% isopropanol in hexane, 0.1% aqueous diethyl amine, 0.1% or 0.2% 2,6-diethylaniline in tert butyl methyl ether. Peaks were detected at 220 and 254 nm.
Example 124
The R and S enantiomers of racemic compounds and the diastereomers (including cis- and trans-) of compounds were separated using either Chiral SFC or Chiral HPLC or preparative HPLC or SFC utilizing different columns such as XBridge Shield RP18 OBD, (CHIRALCEL OJ, CHIRALCEL OD, ChiralPAK AD, (R,R)-WHELK-O1-Kromasil, ChiralPAK IA, ChiralPAK IC, ChiralPAK ID, Lux Cellulose-4, SHIMADZU-SPD-20A, Phenomenex Lux, Cellulose-4, Amchemteq AC1 Am-1 with different dimensions and diameter.
Columns were eluted with two mobile phases (Phase A and Phase B) with gradient from 0 to 100% for both phases. Some examples of phases used but not limited: 0.1% diethylamine in MeOH, water (0.05% TFA), MeCN, Hexane (0.1% diethylamine or diisopropylamine), MeOH, dichloromethane, isopropanol, ethanol, MTBE, 0.2% isopropanol in EtOH, 0.1% isopropanol in hexane, 0.1% aqueous diethyl amine, 0.1% or 0.2% 2,6-diethylaniline in tert butyl methyl ether. Peaks were detected at 220 and 254 nm.
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