A synthetic procedure was developed to prepare dual acid–base catalysts on a single platform. Mesoporous SBA-15 was derivatized using known grafting chemistry via the following steps: (1) addition of Boc-protected 3-aminopropyltriethoxysilane; (2) controlled use of UV/ozonolysis to selectively remove the exterior groups; (3) decoration of the exterior sites freed in Step 2 with 3-mercaptopropyltriethoxysilane; (4) selective oxidation of the mercaptan groups to sulfonic acid; and (5) pyrolytic deprotection of the amine. The resulting catalysts contain sulfonic acid functionality on the external surfaces and entrance of the pores and amino groups deep inside those pores, at coverage ratios that can be controlled by tuning the exposure time during the UV/ozonolysis step. The samples were fully characterized by ²⁹Si and ¹³C solid-state NMR, infrared absorption spectroscopy, acid–base titrations, and N₂ adsorption isotherms measurements, and they were successfully tested for the promotion of a cascade Henry reaction. Optimum performance was seen with the catalyst having an overall 1:2 acid:base molar ratio.

中文翻译：

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具有空间分辨的酸性和基本分子功能的固体催化剂的合成

开发了一种合成程序，可以在一个平台上制备双酸碱催化剂。使用已知的接枝化学方法，通过以下步骤将中孔SBA-15衍生化：（1）添加Boc保护的3-氨丙基三乙氧基硅烷；（2）有控制地使用紫外线/臭氧分解法有选择地除去外部基团；（3）用3-巯基丙基三乙氧基硅烷装饰步骤2中释放的外部部位；（4）将硫醇基团选择性氧化为磺酸；（5）胺的热解脱保护。所得催化剂在孔的外表面和孔的入口处具有磺酸官能度，并且在孔的深处具有氨基，其覆盖率可通过调节UV /臭氧分解步骤中的曝光时间来控制。样品被充分表征为²⁹Si和¹³ C固态NMR，红外吸收光谱法，酸碱滴定法和N ₂吸附等温线测量，它们已成功测试了促进级联亨利反应的能力。对于具有总的1：2的酸：碱摩尔比的催化剂，可以看到最佳性能。