Efficient and mild muscone preparing method

Efficient and mild muscone preparing method

  • CN 104,529,731 A
  • Filed: 01/07/2015
  • Published: 04/22/2015
  • Est. Priority Date: 01/07/2015
  • Status: Active Application
First Claim
Patent Images

1. efficient gentleness prepares a method for muskone, it is characterized in that, with pentadecane diprotic acid for the method for muskone to be prepared by raw material by esterification, acyloin condensation reaction, eliminative reaction, Michael reaction;

  • Specifically comprise the following steps;

    (a), with pentadecane diprotic acid for raw material, sulfuric acid is catalyzer, with ethanol generation esterification, obtains pentadecane binary acids diethyl esters;

    Wherein temperature of reaction is 60 DEG C-90 DEG C, and the reaction times is 12-24 hour;

    (b), under the protection of nitrogen, sodium Metal 99.5 is made sodium sand by heated and stirred in toluene solution, and prepare pentadecane binary acids diethyl esters generation acyloin condensation in step (a) and react, obtained 2-hydroxyl cyclopentadecanone;

    Wherein temperature of reaction is 100 DEG C-130 DEG C, and the reaction times is 6-12 hour;

    (c), obtain E-2-cyclopentadecylene ketone solution by there is eliminative reaction in Burgess reagent dropwise to the diethyl ether solution of the 2-hydroxyl cyclopentadecanone in step (b), wherein the temperature of reaction of eliminative reaction is 15 DEG C-30 DEG C, and the reaction times is 10-24 hour;

    D (), E-2-cyclopentadecanone solution step (c) prepared slowly are added drop-wise in lithium dimethylcuprate solution and Michael reaction occurs obtain muskone;

    Wherein temperature of reaction is-30 DEG C--15 DEG C, the reaction times is 10-24 hour.

View all claims
    ×
    ×

    Thank you for your feedback

    ×
    ×