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ChemicalBook CAS DataBase List Cycloheptanol

Cycloheptanol synthesis

9synthesis methods
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Yield:111-16-0 8.6% ,502-42-1 7.3% ,502-41-0 18.2%

Reaction Conditions:

with polytetrafluoroethylene;cobalt(II) 5,10,15,20-tetra(4'-chlorophenyl)porphyrinate;oxygen at 20 - 120; under 7500.75 Torr; for 8 h;Autoclave;Cooling with ice;Temperature;Pressure;Reagent/catalyst;

Steps:

1-13 Example 9
In a 100 mL stainless steel autoclave with a tetrafluoroethylene liner, 1.0 mg of 5,10,15,20-tetrakis(p-chlorophenyl)porphyrin cobalt (II) was dissolved in 50.0 g of cycloheptane to block the high pressure. kettle.Stir the temperature to 120 ° C,Passing O2 to 1.0 MPa, stirring the reaction at 120 ° C, 1.0 MPa O 2 pressure for 48.0 h,Stir in the ice water bath and cool to room temperature.Turn on the autoclave,The resulting reaction mixture was filtered,The obtained solid was washed with 3×10 mL of cycloheptane and dried under vacuum at 60 ° C.Obtained 6.88g of white solid, which is pimelic acid.The yield was 8.6%.Filtration of the filtrate obtained by filtration,Take the fraction of 179 ° C ~ 180 ° C 10.39g,That is cyclohexanone, the yield is 18.2%;Take 5.2 ° C ~ 186 ° C fraction 5.24g,That is cycloheptanol,Yield 7.3%;At the same time, unreacted cycloheptane is recovered by rectification.

References:

Zhejiang University of Technology;She Yuanbin;Deng Jinhui;Shen Haimin CN109438176, 2019, A Location in patent:Paragraph 0015; 0016; 0017; 0018; 0019; 0020; 0021-0040

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