High-performance liquid chromatographic separation of monoalkylglycerol enantiomers on a chiral stationary phase.
High-performance liquid chromatographic separation of monoalkylglycerol enantiomers on a chiral stationary phase.
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手性固定相上单烷基甘油对映体的高效液相色谱分离。
DOI：
10.1016/s0021-9673(01)93501-0
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发表时间：
1986
期刊：
影响因子：
--
通讯作者：
Y. Itabashi
中科院分区：
文献类型：
--
作者：
T. Takagi;Y. Itabashi
加入400 μ l无水甲苯、1 mg异氰酸3，5-二硝基苯酯（Sumitomo，Osaka，Japan）和40 μ l无水吡啶。将混合物在0.5ml玻璃小瓶中在70 ℃下保持1小时，该玻璃小瓶具有PTFE连接的螺旋盖，偶尔摇动。冷却后，在40 ℃下减压除去溶剂.在含有荧光指示剂（Analtech，纽瓦克，DE，美国）的硅胶GF板（20 cm × 20 cm，厚度0.25 mm）上通过TLC纯化所得的洗脱液。使用前，用氯仿显色，然后在110 -120 ℃活化3小时.将溶解在1 ml氯仿中的反应混合物点样，并用正己烷-1，2-二氯乙烷∶乙醇（40 ∶ 10 ∶ 2）展开两次。在紫外光照射下标记该吸收带（Rp0.4 -0.5），并用乙醚从吸附剂中提取。
452 NOTES400 pl of dry toluene, and 1 mg of 3, 5-dinitrophenyl isocyanate (Sumitomo, Osaka, Japan) and 40~ 1 of dry pyridine were added. The mixture was kept at 70 C for 1 h in a 0.5 ml glass vial with a PTFE-linked screw-cap with occasional shaking. After cooling, the solvent was removed at 40 C under reduced pressure. The resulting urethanes were purified by TLC on a silica gel GF plate (20 cm x 20 cm, thickness 0.25 mm) containing a fluorescence indicator (Analtech, Newark, DE, USA). Prior to use, the plate was developed with chloroform and then activated at 1 lo-120 C for 3 h. The reaction mixture dissolved in 1 ml of chloroform was spotted and developed twice using n-hexane-1, 2-dichloroethaneeethanol(40: 10: 2). The band of the urethanes (Rp 0.4-0.5) was marked under UV irradiation, and extracted from the adsorbent with diethyl ether.