2-ACETYLCYCLOHEXANONE synthesis
- Product Name:2-ACETYLCYCLOHEXANONE
- CAS Number:874-23-7
- Molecular formula:C8H12O2
- Molecular Weight:140.18
Yield:874-23-7 95%
Reaction Conditions:
Stage #1:cyclohexanone with lithium diisopropyl amide in tetrahydrofuran at 0 - 20; for 1.5 h;
Stage #2:acetyl chloride in tetrahydrofuran at 20; for 2 h;Cooling with ice;Temperature;Solvent;Reagent/catalyst;
Steps:
1
1) 3.4 mL of cyclohexanone was added to 25 mL of re-distilled tetrahydrofuran, cooled to 0-5 ° C with an ice-water bath, 20 mL of lithium diisopropylamide at a concentration of 2 mol / L was added dropwise,And then remove the ice bath, stirring at room temperature for 1.5h;(2) 9.8 mL of 8 mol / L acetyl chloride in chloroform was added dropwise to the reaction system of step (1) under ice-water bath condition, and then the ice-water bath was removed and stirred for 2 h at room temperature.(3) The product in step (2) was washed twice with water, and then the chloroform in the separated oil phase was spin-dried using a rotary evaporator, and then vacuum distilled under reduced pressure, vacuum degree of vacuum distillation Was -0.960 MPa, the fraction of 118-136 ° C was collected in 3.2 mL, and the resulting fraction was 2-acetylcyclohexanone in a yield of 95%.
References:
Nanjing University of Technology;HAN, GUOZHI;LIU, DANDAN;WANG, YU;LI, SEN CN106083554, 2016, A Location in patent:Paragraph 0009; 0024-0027
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