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Preparation method of 3-methyl-2-butene-1-aldehyde diisopentenyl acetal

A technology of aldehyde di-prenyl acetal and prenyl alcohol, which is applied in the field of preparation of 3-methyl-2-butene-1-aldehyde di-prenyl acetal, can solve the problem of citral Problems such as the influence of the selectivity and yield of the condensation reaction of intermediates, to achieve the effect of improving selectivity, reducing side reactions, and increasing economic benefits

Active Publication Date: 2022-04-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In summary, in the current synthetic method of 3-methyl-2-butene-1-aldehyde di-prenyl acetal, the citral intermediate in the prenyl alcohol is not considered to affect the selectivity and yield of the condensation reaction. rate impact

Method used

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  • Preparation method of 3-methyl-2-butene-1-aldehyde diisopentenyl acetal
  • Preparation method of 3-methyl-2-butene-1-aldehyde diisopentenyl acetal

Examples

Experimental program
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Effect test

Embodiment 1

[0041]300 g of prenyl alcohol content of 63 wt%, prenyl aldehyde content of 35 wt%, 2,4,4-trimethyl-3-formyl-1,5-hexadiene content of 2 wt% isopentene After the content of alcohol B and 1050g 2,4,4-trimethyl-3-formyl-1,5-hexadiene is 4wt% isopentenol C mixed (the mass ratio of two flows of B and C is 0.3:1.05), into the water azeotropic rectification column for purification. The water consumption is 675g, which is 50wt% of the total mass of the mixture of prenyl alcohols B and C, operated at normal pressure, and the number of packing plates in the azeotropic separation tower is 20, and the mixture of prenyl alcohols B and C is in the rectification tower The upper part of the feed, the feed rate is 2.5g / min, water is fed in the lower part of the rectification tower, the feed rate is 1.25g / min, the temperature at the top of the tower is 94°C, and the temperature at the bottom of the tower is 101°C ; After the steam at the top of the rectification tower is condensed, the phase s...

Embodiment 2

[0046] 9000g of isoamyl alcohol with 89.5wt% prenol, 10wt% prenal and 0.5wt% 2,4,4-trimethyl-3-formyl-1,5-hexadiene After the content of pentenol B and 990g 2,4,4-trimethyl-3-formyl-1,5-hexadiene is 1wt% prenol C after mixing (the mass of B, C two flows Ratio is 9:0.99), enters the water azeotropic rectification tower to carry out purification. The water consumption is 999g, which is 10wt% of the total mass of the mixture of prenyl alcohols B and C, operated at normal pressure, and the number of packing plates in the azeotropic separation tower is 25, and the mixture of prenyl alcohols B and C is in the rectification tower The upper part of the feed is fed at a feed rate of 2.5g / min, water is fed at the lower half of the rectification tower, the feed rate is 0.25g / min, the temperature at the top of the tower is 96°C, and the temperature at the bottom of the tower is 103°C ; After the steam at the top of the rectification tower is condensed, the phase separation is carried out...

Embodiment 3

[0051] 4500g of prenol content of 76.25wt%, prenyl aldehyde content of 22.50wt%, 2,4,4-trimethyl-3-formyl-1,5-hexadiene content of 1.25wt% The content of isopentenol B and 1020g 2,4,4-trimethyl-3-formyl-1,5-hexadiene is 2.5wt% after mixing prenol C (B, C two flows The mass ratio is 4.5:1.02), enters the water azeotropic rectification column and purifies. The water consumption is 1656g, which is 30wt% of the total mass of the prenol mixture B and C after mixing, operated under normal pressure, and the packing plate number of the azeotropic separation tower is 15, and the mixture of prenol B and C in the rectification tower The upper part of the feed, the feed rate is 2.5g / min, water is fed in the lower part of the rectification tower, the feed rate is 0.75g / min, the temperature at the top of the tower is 95 ° C, and the temperature of the bottom of the tower is 102 ° C ; After the steam at the top of the rectification tower is condensed, the phase separation is carried out in ...

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Abstract

The invention provides a preparation method of 3-methyl-2-butene-1-aldehyde diisopentenyl acetal and a preparation method of the 3-methyl-2-butene-1-aldehyde diisopentenyl acetal. According to the method, the isopentenol in which the content of 2, 4, 4-trimethyl-3-formyl-1, 5-hexadiene is controlled to be 0.001-0.05 wt% is used as a raw material, so that side reactions in the condensation reaction process can be effectively reduced, the selectivity of the 3-methyl-2-butene-1-aldehyde diisopentenyl acetal is improved by more than or equal to 5% in terms of the isopentenol, and the economic benefit is remarkably increased.

Description

technical field [0001] The invention belongs to the field of synthesis of fine chemicals, and in particular relates to a preparation method of 3-methyl-2-butene-1-aldehyde di-isopentenyl acetal. Background technique [0002] 3-Methyl-2-butene-1-aldehyde diisopentenyl acetal is an important intermediate in the synthesis of citral, and as a key raw material for flavors, fragrances and nutritional chemicals, citral is widely used in the synthesis of fragrances (holol , geraniol, nerol, citronellol, lily of the valley pyran) and nutritional products (vitamin A, vitamin E, carotenoids), etc., have important commercial value. [0003] In US4133836A, nitric acid (concentration is 1×10 -6 ~1wt%) is used as a catalyst to prepare 3-methyl-2-butene-1-aldehyde diisopentenyl acetal by reactive distillation process, the reaction pressure is 2-200mmHg (absolute pressure), and the temperature is 15-100°C . US2002035298A1 improves US4133836A by using a secondary evaporation device for the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/56C07C41/58C07C43/303
Inventor 刘英俊孙钦鹤张永振张红涛朱小瑞庞计昌沈元伟
Owner WANHUA CHEM GRP CO LTD
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