In this report the synthesis and characterization of chiral stationary phase of cellulose tris(3,5 dimethylphenylcarbamate) coated zirconia(CDMPC ZrO 2 CSP) was described. Direct optical resolutions of acidic racemate...In this report the synthesis and characterization of chiral stationary phase of cellulose tris(3,5 dimethylphenylcarbamate) coated zirconia(CDMPC ZrO 2 CSP) was described. Direct optical resolutions of acidic racemate naproxen and its derivatives on the phase were investigated. Surface property of zirconia affects the chiral separation of naproxen greatly. Naproxen could not be eluted from the column unless an acidic modifier was present in the mobile phase. However, good chiral resolutions were obtained for its ester derivatives. The influences of loading amount of stationary phase, molecular structure of compounds, type of alcohols as the modifier and their concentration in mobile phase on chiral resolution were studied. The chiral recognition mechanism of the chiral stationary phase was discussed.展开更多
The present paper covers a novel method for the preparation of α-naphthylacetone via the addition-hydrolysis reaction of a 2-（α-naphthylmethyl）benzimidazolium salt with Grignard reagent.The IR spectrum,MS and 1H N...The present paper covers a novel method for the preparation of α-naphthylacetone via the addition-hydrolysis reaction of a 2-（α-naphthylmethyl）benzimidazolium salt with Grignard reagent.The IR spectrum,MS and 1H NMR of the title compound are consistent with those reported.This method provides a convenient and inexpensive access to the title compound.The mechanism for the addition-hydrolysis reaction of benzimi-（dazolium） salt with Grignard reagent and the effects of reaction conditions on the yield are discussed.展开更多
文摘In this report the synthesis and characterization of chiral stationary phase of cellulose tris(3,5 dimethylphenylcarbamate) coated zirconia(CDMPC ZrO 2 CSP) was described. Direct optical resolutions of acidic racemate naproxen and its derivatives on the phase were investigated. Surface property of zirconia affects the chiral separation of naproxen greatly. Naproxen could not be eluted from the column unless an acidic modifier was present in the mobile phase. However, good chiral resolutions were obtained for its ester derivatives. The influences of loading amount of stationary phase, molecular structure of compounds, type of alcohols as the modifier and their concentration in mobile phase on chiral resolution were studied. The chiral recognition mechanism of the chiral stationary phase was discussed.
文摘The present paper covers a novel method for the preparation of α-naphthylacetone via the addition-hydrolysis reaction of a 2-（α-naphthylmethyl）benzimidazolium salt with Grignard reagent.The IR spectrum,MS and 1H NMR of the title compound are consistent with those reported.This method provides a convenient and inexpensive access to the title compound.The mechanism for the addition-hydrolysis reaction of benzimi-（dazolium） salt with Grignard reagent and the effects of reaction conditions on the yield are discussed.
