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Synthetic method of polysantol

A technology of dosanol and trimethyl, which is applied in the field of preparation of dosanol, can solve problems such as separation, recovery and recycling difficulties, environmental hazards, cumbersome operation, etc., and achieve good thermal and chemical stability, and usage The effect of less and simple operation

Active Publication Date: 2015-06-10
ZHEJIANG XINHUA CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional quaternary ammonium salt phase transfer catalyst has poor thermal stability, separation, recovery and recycling are difficult, so its use has been restricted to a certain extent.
And this reaction uses a large amount of toxic organic solvents, which causes harm to the environment, and makes the operation cumbersome and the post-processing complicated.

Method used

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  • Synthetic method of polysantol
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: Preparation of 3-methyl-5-(2,2,3-trimethyl-3-cyclopentenyl)-3-penten-2-one

[0020] Add 9mol methyl ethyl ketone, 40mol methanol, 0.9mol KOH to the reaction kettle, add 4.6mol borneolenal dropwise under stirring, the reaction temperature is 28~35°C, drop it in 8~10 hours, and continue to react for 2~3 hours until the reaction completely. Then neutralize with acetic acid, then wash with water until neutral. Remove the solvent methanol and unreacted butanone, and distill under reduced pressure to obtain 865.2 g of product with a yield of 92%.

Embodiment 2

[0021] Example 2: Preparation of 3,3-dimethyl-5-(2,2,3-trimethyl-3-cyclopentenyl)-4-penten-2-one

[0022] Add 1mol of 3-methyl-5-(2,2,3-trimethyl-3-cyclopentenyl)-3-penten-2-one and 0.5mol of NaOH to the reaction kettle, stir rapidly after mixing, 0.5mol ionic liquid [(n-C 4 h 9 ) 4 N][PF 4 ], 1.5mol CH 3 1, continue to stir for 2-5 hours after dropping, finish the reaction. The reaction system is divided into two layers, the upper layer is 3,3-dimethyl-5-(2,2,3-trimethyl-3-cyclopentenyl)-4-penten-2-one crude product, the lower layer is ionic liquid. The upper layer was neutralized with acetic acid and washed with water to become neutral, and the unreacted raw materials were removed by distillation under reduced pressure to obtain 187.8 g of the product with a yield of 85%.

Embodiment 3

[0023] Example 3: Preparation of 3,3-dimethyl-5-(2,2,3-trimethyl-3-cyclopentenyl)-4-penten-2-one

[0024] Add 3-methyl-5-(2,2,3-trimethyl-3-cyclopentenyl)-3-penten-2-one 1mol to the reaction kettle, Cs 2 CO 3 0.5mol, stir rapidly after mixing, drop 0.5mol ionic liquid at room temperature [(n-C 4 h 9 ) 4 N][PF 4 ], 1.5mol CH 3 1, continue to stir for 2-5 hours after dropping, finish the reaction. The reaction system is divided into two layers, the upper layer is 3,3-dimethyl-5-(2,2,3-trimethyl-3-cyclopentenyl)-4-penten-2-one crude product, the lower layer is ionic liquid. The upper layer was neutralized with acetic acid, washed with water to become neutral, and unreacted raw materials were removed by distillation under reduced pressure to obtain 190.7 g of product with a yield of 86.3%.

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Abstract

The invention relates to a synthetic method of polysantol. According to the synthetic method, campholenic aldehyde is taken as a raw material; campholenic aldehyde and butanone are subjected to aldol condensation; then methylation is performed using a solid alkali and an ionic liquid as phase transfer catalysts so as to obtain 3, 3-dimethyl-5-(2, 2, 3-trimethyl-3-cyclopentenyl)-4-pentene-2-one; and at last reduction is performed using sodium borohydride, and finished products are obtained after rectification. Advantages of the synthetic method are that: the ionic liquid is used as the phase transfer catalyst, so that using of organic solvents is avoided. Compared with traditional phase transfer catalysts, ionic liquid possesses excellent heat stability and chemical stability, application amount is less, toxicity is low, operation is simple, and ionic liquid can be recycled.

Description

technical field [0001] The invention relates to a perfume synthesis method in the technical field of chemical industry, in particular to a preparation method of dosantol. Background technique [0002] As one of the oldest and most valuable spices, sandalwood was originally extracted from natural sandalwood by East Indians. In modern times, due to the rapid increase in the consumption of daily chemical flavors and fragrances, natural sandalwood is far from meeting the market demand. The development of modern synthesis technology provides people with rich and sufficient fragrance products, ushering in a new era for the flavor and fragrance industry. Sandalwood, as a kind of precious sandalwood, has a stable chemical structure, so that it has a long-lasting, mild, sweet aroma, and is widely used in the field of daily chemical essence. Dalsantol, Chinese name 3,3-dimethyl-5-(2,2,3-trimethyl-3-cyclopentenyl)-4-penten-2-ol, English name 3,3- dimethyl-5-(2,2,3-trimethyl-3-cyclope...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C33/12C07C29/143C07C49/21C07C45/68
CPCC07C29/143C07C45/68C07C45/74C07C2601/10C07C33/12C07C49/21
Inventor 包江峰谢海英王卫明谢自强陈宏徐利红应登宇赵建标柯美生唐一前
Owner ZHEJIANG XINHUA CHEM