核磁共振技术测定联萘酚的对映体纯度
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奚忠华, 陆大东, 戴洁, 叶涛, 章文伟
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Determination of Enantiomeric Purity of Binaphthol by NMR Method
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Zhonghua Xi, Dadong Lu, Jie Dai, Tao Ye, Wenwei Zhang
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表2 联萘酚手性液相色谱方法与核磁共振方法(R)-BINOL含量和ee值测定结果
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| No. | R : S | ee | HPLC | | 1H NMR, a | | 1H NMR, b | | 1H NMR, c | | R% | ee | R% | ee | R% | ee | R% | ee | | 1 | 90 : 10 | 80% | 88.9% | 77.8% | | 88.6% | 77.2% | | 88.7% | 77.5% | | 87.8% | 75.5% | | 2 | 80 : 20 | 60% | 79.3% | 58.6% | | 78.9% | 57.8% | | 79.6% | 59.3% | | 77.6% | 55.2% | | 3 | 70 : 30 | 40% | 68.1% | 36.2% | | 68.4% | 36.8% | | 69.6% | 39.3% | | 66.4% | 32.8% | | 4 | 40 : 60 | 20% | 59.2% | 18.4% | | 59.0% | 18.0% | | 59.4% | 18.8% | | 55.6% | 11.3% | | 5 | 50 : 50 | 0% | 49.7% | ?0.6% | | 49.3% | ?1.4% | | 49.6% | ?0.7% | | 45.9% | ?8.2% | | 6 | 40 : 60 | ?20% | 39.8% | ?20.4% | | 39.3% | ?21.4% | | 40.4% | ?19.1% | | 37.5% | ?25.0% | | 7 | 30 : 70 | ?40% | 29.9% | ?40.2% | | 29.4% | ?41.2% | | 29.3% | ?41.4% | | 26.6% | ?46.7% | | 8 | 20 : 80 | ?60% | 19.9% | ?60.2% | | 19.8% | ?60.4% | | 20.3% | ?59.4% | | 17.9% | ?64.1% | | 9 | 10 : 90 | ?80% | 9.7% | ?80.6% | | 9.9% | ?80.2% | | 9.9% | ?80.3% | | 8.4% | ?83.2% |
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