CYCLOHEXANOL-D12 synthesis

Yield:66522-78-9 12 %Chromat.

Reaction Conditions:

with C₁₉H₂₂N₄O₄^(4-)*Co⁽³⁺⁾*Li⁽¹⁺⁾;3-chloro-benzenecarboperoxoic acid in dichloromethane;propan-2-one at 25; for 0.5 h;Catalytic behavior;Inert atmosphere;Sealed tube;

Steps:

Catalytic reaction conditions and productanalysis

General procedure: A 5.0 ml vial containing solution of 1 and substrate in acetone:CH2Cl2 (vol/vol = 1:3) and another vial containingm-CPBA in acetone:CH2Cl2 (vol/vol = 1:3), were sealedusing rubber septum and purged under an Ar atmosphereat 25 °C for 30 min. The solution containing m-CPBA was then taken out and injected into the reactionvial containing 1 and substrate via gas tight syringe andstirred under an Ar atmosphere for 30 min. The final concentrationsof 1, m-CPBA, and substrates were 0.10 mM,5.0 mM, and 0.50 M, respectively. The same reaction conditions,but in the presence of CCl3Br (5.0 mM) under anAr atmosphere and in the absence and presence of CCl3Br(5.0 mM) under an O2 (or air) atmosphere were also used.After 30 min, products formed in the oxidation of substrates,such as cyclohexane, cyclohexene, styrene, cis-stilbene,trans-stilbene, and anthracene, by 1 and m-CPBAwere analyzed by GC and GC-MS. The inorganic cobaltproducts obtained in the oxidation of substrates by 1 andm-CPBA were also analyzed by EPR and ESI-MS.

References:

Malik, Deesha D.;Lee, Yong-Min;Nam, Wonwoo [Bulletin of the Korean Chemical Society,2022,vol. 43,# 8,p. 1075 - 1082] Location in patent:supporting information