The Research On Asymmetric Synthesis And Crystal Structure Of3,5-dimethyl-2-(3-fluorinephenyl)-2-morpholinol Hydrochloride

The subject in the previous synthesis, racemic compounds of3,5-dimethy-2-（3-fluorinephenyl）-2-morpholinol hydrochloride. Enantiopure （2R,3R,5S）-3,5-dime-thy-2-（3-fluorinephenyl）-2-morpholinol hydrochloride （4A） and （2S,3S,5R）-3,5-dimethy-2-（3-fluorinephenyl）-2-morpholinol hydrochloride（4B） was synthesizedfrom （S）-2-amino-propanol and2-bromo-m-fluorinephenone,（R）-2-amino-propanoland2-bromo-m-fluorine-phenone., the single crystal growing method of slowevaporation of the solvent, a mixed solvent consisting of anhydrous ethanol, etc. avariety of organic solvents. X single crystal diffraction determination of the crystalstructure of this chiral enantiomer compounds and the spatial structure of twocompounds, and preliminary analysis of the space of two compounds synthesismechanism.Colorless single crystal cultivate a mixed solvent such as ethanol, RigakuSaturn724CCD X-ray single-crystal diffractometer with monochromatic Mo Karadiation source （λ=0.071073nm）, temperature113（2） K,ω-Ф scan mode to collectdiffraction data. Restore the indicators Saint procedures diffraction data, SHELXL-97program, the single crystal structure analysis, using the method of least squaresprogram SHELXL-97（F²fine repair）. Determined by single-crystal X-ray diffractionmeasurement of the relative position of each atom of the compound to obtain acompound of the formula C₁₂H₁₇ClFNO₂.Using single-crystal X-ray analysismeasured by crystal structure and space structure.The compound4A crystal belongsto orthorhombic system with space group P21212and cell parameters:a=8.6886（12）nm, b=20.059（3） nm,c=7.6052（9） nm, Z=4, V=1.3255（6） nm³, Dc=1.311g/cm³,F（000）=552, R₁=0.0257, wR₂=0.0650, S=1.021.The compound4B crystal belongs to orthorhombic system with space group P2₁2₁2and cell parameters:a=8.6887（9）nm,b=20.064（2） nm, c=7.6135（7） nm, Z=4, V=1.3272（3） nm³, Dc=1.310g/cm³,F（000）=552, R₁=0.0356, wR₂=0.0653, S=1.033.This expriment has no special catalyst, without complex split expriment,stereoselective high optical purity. It is a simple chiral pure compounds.