Synthesizing method of 2-butyl-1-octanol

A synthesis method, butyl technology, applied in the preparation of carbon-based compounds, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve problems such as expensive catalysts

Inactive Publication Date: 2018-06-22
福建未来药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the catalyst for this preparation method is relatively expensive, and it is currently limited to the stage of small experiments.
The last one is to place n-hexanal in a supercritical carbon dioxide solvent, in SiO 2 Surface-attached NMAP (N-methylpropylamine) is pressurized to 22.9MPa to obtain the product. This method is a green and non-polluting method that represents the direction of future research, but it is currently limited to the research stage of the laboratory.

Method used

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  • Synthesizing method of 2-butyl-1-octanol
  • Synthesizing method of 2-butyl-1-octanol

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Such as figure 1 Shown is the reaction equation of aldol condensation reaction, and concrete process is as follows: Hexanal (13.9g) adds the aqueous solution of barium hydroxide (2.2g Ba(OH) 2 .8H 2 (0, 25ml of water), heating to reflux for 1 hour, liquid separation, and vacuum distillation to collect 70-80°C (310Pa) fractions to obtain 2-butyl-2-octenal (20.3g).

[0022] Such as figure 2 Shown is the reaction equation of primary reduction reaction and secondary reduction reaction of the present invention, concrete process is as follows: the above-mentioned 2-butyl-2-octenal that obtains is dissolved in methanol (160ml), adds palladium carbon (2.031g, 5 %Pd / C), replace the air with vacuum, pressurize (1.5MPa), heat the temperature to 100°C, the raw material is converted into a mixture of aldehyde and alcohol, and this mixture of aldehyde and alcohol is added with NaBH 4 (3.0g) reduction, react at room temperature (25°C) for 1 hour, heat up to 50°C, add water (100ml)...

Embodiment 2

[0024] Hexanal (123ml, 100.1g) was placed in a 1000ml three-necked flask, and an aqueous solution of barium hydroxide (8.9g Ba(OH) 2 .8H 2 (2, 100ml water), dripped in about 20 minutes, heated to reflux for 1 hour, and separated liquids, and the organic layer obtained was collected by distillation under reduced pressure at 70-80°C (310Pa) cuts to obtain 2-butyl-2-octenal ( 163.9g).

[0025] The 2-butyl-2-octenal obtained above was dissolved in methanol (320ml), palladium carbon (8.15g, 5% Pd / C) was added, the air was replaced by vacuum, pressurized (1MPa), and the temperature was heated to 50°C. Converted to a mixture of aldehydes and alcohols, this mixture of aldehydes and alcohols is added with NaBH 4 (30.7g) was reduced, heated to 50°C, added water (200ml) after 1 hour, stirred for 15 minutes, concentrated methanol under reduced pressure, added saturated brine (400ml), extracted twice with ethyl acetate, and combined the ethyl acetate layers , spin-dried under reduced pr...

Embodiment 3

[0027] Hexanal (3.8L, 3.1kg) was placed in a 20L reaction flask, and an aqueous solution of barium hydroxide (170.2g Ba(OH) 2 .8H 2 O, 2.5L water), about 1 hour drop, heated to reflux for 1 hour, liquid separation, the upper layer vacuum distillation collected 70-80 ° C fraction (310Pa), to obtain 2-butyl-2-octenal (5.0kg) .

[0028] The above-mentioned 2-butyl-2-octenal was dissolved in methanol (8.0L), and palladium carbon (24.9g, 5% Pd / C) was added, the air was replaced by vacuum, pressurized (1MPa), and the temperature was heated to 50°C. Converted to a mixture of aldehydes and alcohols, this mixture of aldehydes and alcohols is added with NaBH 4 (93.6g) reduction, no obvious bubbles, heated to 50 ° C, added water (600ml) after 1 hour, stirred for 15 minutes, concentrated methanol under reduced pressure, added brine (1000ml), extracted twice with ethyl acetate, combined ethyl acetate The ester layer was spin-dried under reduced pressure, distilled by an oil pump under r...

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Abstract

The invention discloses a synthesizing method of 2-butyl-1-octanol. The method includes the following steps of conducting an aldol condensation reaction with n-caproaldehyde as the initiator to obtain2-butyl-2-octenal, wherein a catalyst in the aldol condensation reaction is barium hydroxide; conducting a primary reduction reaction on 2-butyl-2-octenal to obtain a mixture of aldehyde and alcohol,and conducting a secondary reduction reaction on the mixture of aldehyde and alcohol to obtain 2-butyl-1-octanol, wherein a reducing agent in the primary reduction reaction is palladium on carbon, and a reducing agent in the secondary reduction reaction is sodium borohydride. The method is easy to operate, few byproducts are produced, yield is high, the requirements for devices are not high, andindustrial production is easy.

Description

technical field [0001] The invention relates to a synthesis method of 2-butyl-1-octanol, which belongs to the technical field of chemical industry. Background technique [0002] At present, 2-butyl-1-octanol is a key intermediate in the synthesis of optoelectronic materials, and its batch synthesis has become a key step for the industrial production of optoelectronic materials. There are several methods for preparing 2-butyl-1-octanol: a method of reducing alcohol by acid or ester, although the reduction yield of this step can reach 95%, but because the raw material acid is not easy to obtain, its amplification Production is limited; the second is by n-hexanol in an IrCl(COD) 2 It can be obtained under the action of catalyst and KOH alkaline condition. However, the catalyst for this preparation method is relatively expensive, and it is currently limited to the stage of small experiments. The last one is to place n-hexanal in a supercritical carbon dioxide solvent, in SiO ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/17C07C31/125
CPCC07C29/172C07C45/74C07C31/125C07C47/21
Inventor 姜冉连福寿魏初铨
Owner 福建未来药业有限公司
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