614-45-9Relevant articles and documents
Immobilization of (l)-valine and (l)-valinol on SBA-15 nanoporous silica and their application as chiral heterogeneous ligands in the Cu-catalyzed asymmetric allylic oxidation of alkenes
Ashouri, Akram,Mahramasrar, Mahsa,Majidian, Shiva,Rashid, Hersh I,Samadi, Saadi
supporting information, p. 17630 - 17641 (2021/10/04)
SBA-15 nanoporous silica was synthesized by hydrothermal method using P123 surfactant and tetraethoxyortosilicate in acidic condition and then functionalized by 3-chloropropyltrimethoxysilane. Next, by immobilization of chiral amino acid (S)-2-amino-3-methyl butanoic acid (l-valine) and chiral amino alcohol (S)-2-amino-3-methylbutane-1-ol (l-valinol), preparedviathe reduction ofl-valine by NaBH4/I2in THF, on functionalized-SBA-15, chiral heterogeneous ligands AL*-i-Pr-SBA-15 and AA*-i-Pr-SBA-15 were prepared and characterized by FT-IR, XRD, TGA, EDX, SEM, BET-BJH techniques. The asymmetric allylic oxidation of alkenes was done using copper-complexes of these ligands and the as-synthesized peresters. The reactions were optimized by varying various parameters such as temperature, solvent, amount of chiral heterogeneous ligand, as well as the type and amount of copper salt. Under optimized conditions, 6 mg of AL*-i-Pr-SBA-15 and 3.2 mol% of Cu(CH3CN)4PF6in acetonitrile at 50 °C, the chiral allylic ester was obtained with 80% yield and 39% enantiomeric excess in 24 h. The recyclability of the chiral heterogeneous catalysts was also evaluated without significant reduction in the reaction results up to three runs.
Preparation method of tert-butyl peroxybenzoate
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Paragraph 0027-0036, (2020/11/05)
The invention discloses a preparation method of tert-butyl peroxybenzoate, specifically comprising the following steps of: salifying tert-butyl hydroperoxide and caustic soda liquid; then dropwise adding benzoyl chloride into sodium tert-butoxide peroxide for coupling, and washing a coupling product twice after liquid separation; and adding a stabilizer into the product, drying, dewatering and carrying out suction filtration to obtain the tert-butyl peroxybenzoate product. The preparation method comprises the following steps of: dropwise adding benzoyl chloride into sodium tert-butoxide peroxide; and after liquid separation, washing with water twice, adding a stabilizer into the upper product phase, adding anhydrous magnesium sulfate for drying, and carrying out suction filtration to obtain tert-butyl peroxybenzoate with the yield of not less than 95% and the content of not less than 99%, so that the product can be stored in a dark place and transported for a long distance.
A Woven Supramolecular Metal-Organic Framework Comprising a Ruthenium Bis(terpyridine) Complex and Cucurbit[8]uril: Enhanced Catalytic Activity toward Alcohol Oxidation
Li, Zhan-Ting,Liu, Yi,Wang, Hui,Wang, Ze-Kun,Xu, Zi-Yue,Zhang, Dan-Wei,Zhang, Yun-Chang
, p. 1498 - 1503 (2020/08/05)
The self-assembly of a diamondoid woven supramolecular metal–organic framework wSMOF-1 has been achieved from intertwined [Ru(tpy)2]2+ (tpy=2,2′,6′,2′′-terpyridine) complex M1 and cucurbit[8]uril (CB[8]) in water, where the intermolecular dimers formed by the appended aromatic arms of M1 are encapsulated in CB[8]. wSMOF-1 exhibits ordered pore periodicity in both water and the solid state, as confirmed by a combination of 1H NMR spectroscopy, UV-vis absorption, isothermal titration calorimetry, dynamic light scattering, small angle X-ray scattering and selected area electron diffraction experiments. The woven framework has a pore aperture of 2.1 nm, which allows for the free access of both secondary and primary alcohols and tert-butyl hydroperoxide (TBHP). Compared with the control molecule [Ru(tpy)2]Cl2, the [Ru(tpy)2]2+ unit of wSMOF-1 exhibits a remarkably higher heterogeneous catalysis activity for the oxidation of alcohols by TBHP in n-hexane. For the oxidation of 1-phenylethan-1-ol, the yield of acetophenone was increased from 10 percent to 95 percent.