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Chemical Structure| 529-02-2 Chemical Structure| 529-02-2

Structure of 529-02-2

Chemical Structure| 529-02-2

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Product Details of [ 529-02-2 ]

CAS No. :529-02-2
Formula : C10H18O
M.W : 154.25
SMILES Code : OC1C(CCC(C)C1)=C(C)C
MDL No. :MFCD08443110

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Application In Synthesis of [ 529-02-2 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 529-02-2 ]

[ 529-02-2 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 106-23-0 ]
  • 2-[2,6-dimethyl-5-heptenyl]-4,4,8-trimethylhexahydro-1,3-benzodioxine [ No CAS ]
  • [ 529-02-2 ]
  • [ 42822-86-6 ]
YieldReaction ConditionsOperation in experiment
<= 7%; <= 10%; 90% sulfuric acid; In water; at 60℃; for 7.0h; A bench-scale PMD synthesis reaction was carried out using a 500 ml jacketed glass reactor, a heated feed vessel, and an over-head stirrer fitted with a four-blade stainless steel impeller, thermometer and two integral baffles. The reactor temperature was set to a temperature of 60 deg C by circulating heating fluid, kept at the desired constant temperature (+/- 0.5 deg C) in a constant temperature bath. Dilute sulphuric acid (14Og of a 0.53% (m/m) solution 0.00757mol) was added to the reactor and allowed to equilibrate to the desired reaction temperature. Citronellal (30.08g; 0.193mol), pre-heated to the desired reaction temperature, was added to the reactor drop-wise over a period of 60 minutes, while the reactor was agitated at a stirring rate of 2000 rpm. The reaction was allowed to proceed for a further 6 hours following completion of the citronellal addition step.Once the reaction had stopped, the reactor contents were drained into a separating funnel and allowed to settle for 1 minute after which the aqueous phase was drained off. The organic phase was washed with 5Og of a 2.5% (w/v) solution of NaHCO3 to remove any residual sulphuric acid catalyst. The mixture was allowed to settle for approximately 2 minutes after which the bottom aqueous phase was drained off.Residual water was removed from the organic phase on a rotary evaporator. The crude product was then distilled under vacuum (1 15 deg C and 8 mBar) to recover citronellal and pulegol. The desired product PMD was recovered as a thick viscous liquid from the bottom of the still and analyzed by means of gas chromatography. In different embodiments, the yield of PMD varied between 80 - 90 % and typically contained up to about 10 % of pulegol, up to about 7% PMD-acetal and about 2- 5% of un-reacted citronellal.
 

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