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Method of preparing citronellol

A technology of citronellol and equation, applied in the field of preparing citronellol, can solve the problems of low efficiency of borane, poor selectivity, impossible to realize industrialization and the like, and achieve the effects of high purity, reduced preparation cost and simple process route

Inactive Publication Date: 2007-08-08
厦门中坤化学有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the poor selectivity of the hydration method, it is impossible to realize industrialization
However, hydroboration has not been a cost-competitive route due to the low efficiency of borane production and the uneconomical hydroboration process.

Method used

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  • Method of preparing citronellol
  • Method of preparing citronellol
  • Method of preparing citronellol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: In a dry three-necked flask equipped with 10ml2.0mol / L boron trifluoride triglyme solution under the protection of a nitrogen atmosphere, 30ml2.0mol / L sodium borohydride triglyme was added dropwise under stirring. Glyme solution and 10ml2.0mol / L aluminum trichloride triglyme solution, the borane produced is introduced into the bottom of the hydroboration reaction bottle through the catheter, and connected to a circular aperture with a diameter of 0.2 The gas disperser of mm is connected, and the drop rate of the reaction liquid is preferably absorbed so that the generated borane can be basically absorbed.

[0030] A mixture of 8 ml of dichloromethane and 25 ml of 85% dihydromyrcene was added to the hydroboration reaction bottle, cooled to 0° C., and the borane produced above was introduced.

[0031] After adding the sodium borohydride solution, after the speed of borane generation slows down, slowly introduce nitrogen gas into the system for 5-20 minutes, put...

Embodiment 2

[0033] Embodiment 2: the difference with Example 1 is that the borohydride used is potassium borohydride, and the end of the bottom gas conduit that imports the borohydrolysis bottle does not have a microporous gas disperser, and the temperature of the borohydride reaction bottle is -14 °C, the reflux time after adding the sodium hydroxide and hydrogen peroxide solution was 2.0 h, and the yield of citronellol was 38%.

Embodiment 3

[0034] Embodiment 3: the difference with Example 1 is that the 2.0mol / L sodium borohydride triglyme solution added in the borane production process is 35ml, and the micropore diameter of the gas disperser used is 0.08mm, in the hydroboration reaction bottle Add a mixed solution of 10ml of dichloromethane and 35ml of 85% dihydromyrcene, the temperature of the hydroboration reaction bottle is -16°C, the reflux time after adding the sodium hydroxide and hydrogen peroxide solution is 2.0h, the citronellol The yield was 87%.

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Abstract

The invention discloses a making method of citronellol, which comprises the following steps: adding solvent in the metal hydroboron powder under nitrogen atmosphere; making hydroboron solution or suspension; sealing; adding solvent in the aluminium chloride under 0 deg.c; making the solution or suspension with density at 0.5-2.0mol / L; sealing; producing borane; hydroborating dimyrcene; decompressing; rectifying to obtain the product.

Description

technical field [0001] The invention relates to an essence, in particular to a method for preparing citronellol by using dihydromyrcene as a raw material. Background technique [0002] Citronellol is an important flavor main product. The existing citronellol production route is mainly obtained from the selective hydrogenation of citral and the reduction of citronellal. The production of citronellol by these two methods has poor economic benefits due to the high price of raw materials. One of the ideal routes for the synthesis of citronellol is the selective hydration or hydroboration of dihydromyrcene, the main product of the cracking of α-pinene, a renewable resource. However, due to the poor selectivity of the hydration method, it is impossible to realize industrialization. Hydroboration, however, has not been a cost-competitive route due to the low efficiency of borane production and the uneconomical hydroboration process. Therefore, exploring an industrial route to pr...

Claims

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Application Information

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IPC IPC(8): C07C33/025C07C29/12
Inventor 杨毅融龚雄辉郑艺辉谢艺雄
Owner 厦门中坤化学有限公司
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