手性樟脑磺酸的合成及表征

以樟脑粉为原料合成了消旋樟脑磺酸;采用l-苯甘氨酸为拆分剂,经拆分、纯化分离得到了手性樟脑磺酸。合成消旋樟脑磺酸的适宜工艺条件为：反应时间25 h,浓硫酸的滴加速度0.5～1.0 mL/min,反应温度10℃,消旋樟脑磺酸的收率85.6%,熔点195～201℃。拆分的适宜工艺条件为：物料比n（dl-樟脑磺酸）∶n（l-苯甘氨酸）=1∶0.95,d-樟脑磺酸拆分收率64%,熔点194～196℃,α]2D0=＋23°（C=5,H2O）;l-樟脑磺酸拆分收率90.8%,熔点197～198℃,α]2D0=-22.5°（C=5,H2O）。样品经熔点、旋光率、红外光谱等检测方法,证明与目标产物一致。

Synthesis and Characterization of Chiral Camphor Sulfonic Acid

The racemic camphor sulfonic acid was synthesized uing camphor powder as the raw material, and chiral camphor sulfonic acid was obtained by splitting, purification and separation. The optimal synthesized condi-tions of racemic camphor sulfonic acid were followings：reaction time was 25 h, the speed of add sulfuric acid was 0. 5 - 1.0 mL ·min-1 ,reaction temperature was 10 ℃ ,the yield of racemic camphor sulfonic was 85.6% ,meltingpoint was 195 -201 ℃. The optimal conditions of resolve were foUowings：materials ratio was n（ racemic camphor sulfonic ） ： n （ l - phenylglycine） = 1 ： 0.95, the yield of d - camphor sulfonic acid was 64 %, melting point was 194- 196 ℃, a] D20 = ＋ 23° （ C = 5, H2O）, and l - camphor sulfonic acid was 90.8%, mehing point was 197 - 198 ℃, a ] D20 = - 22.5° （ C = 5, H2O）. The synthesized products were identified by melting point determination, infra-red spectroscopy （IR） and else analysis methods. The results indicated that they were close to the standard compounds.