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Process for preparing alcohols by hydrolysis of metal-organic products

A metal-organic and product technology, applied in the field of metal-organic product post-processing technology, can solve problems such as product purity decline and hydrolysis process yield decline, and achieve the effects of avoiding halogenated side reactions and improving hydrolysis yield and product content.

Active Publication Date: 2021-04-20
SHANGYU NHU BIOCHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existence of this side reaction often causes the yield of the above-mentioned hydrolysis process to decline or the product purity to decline

Method used

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  • Process for preparing alcohols by hydrolysis of metal-organic products
  • Process for preparing alcohols by hydrolysis of metal-organic products
  • Process for preparing alcohols by hydrolysis of metal-organic products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] The metal-organic product obtained by the Grignard reaction is referred to as the magnesium dichloride condensate for short, and the structure is as follows:

[0048]

[0049] Add 500 mL of an aqueous solution containing 0.3 mol of magnesium bicarbonate into a four-port reactor, then dropwise add 300 mL of an ether solution containing 0.295 mol of magnesium dichloride condensate (this solution also contains 4% of 3-methyl-2-ene- 4-pentynyl alcohol (abbreviated as C6 alcohol, the same below)), the dripping is finished in about 20 minutes, and the hydrolysis reaction is stopped after continuing to stir for 60 minutes. The temperature of the hydrolysis process is controlled between 0 and 20°C. Filtration obtained 49.5 g of solid magnesium carbonate, and the oil-water mixture was separated to obtain 295 mL of ether solution of alcohol products and 490 mL of magnesium salt solution.

[0050] The diethyl ether solution of alcohol products is first reclaimed diethyl ether a...

Embodiment 2

[0059] The metal-organic product obtained by the Grignard reaction is referred to as dibromomagnesium condensate for short, and the structure is as follows:

[0060]

[0061] 500 mL of aqueous solution containing 0.3 mol of magnesium bicarbonate was added to the four-port reactor, and then 300 mL of methyl tetrahydrofuran solution containing 0.295 mol of dibromomagnesium condensate (containing 3% of 3-methyl-2-ene-4 -pentynyl alcohol (abbreviated as C6 alcohol, the same below)), the dripping is completed in about 100 minutes, and then the hydrolysis reaction is stopped after continuing to stir for 10 minutes, and the temperature of the hydrolysis process is controlled between 5 and 25°C. Then it was filtered to obtain 49.4 g of solid magnesium carbonate. The oil-water mixture was separated to obtain 290 mL of a dihydric alcohol solution in methyl tetrahydrofuran and 520 mL of a magnesium salt solution.

[0062] The methyl tetrahydrofuran solution of dibasic alcohol is firs...

Embodiment 3

[0071] The metal-organic product obtained by the ethynylation reaction of methyl ketene is bis(3-methyl-4-yn-1-penten-3-ol) calcium, with the following structure:

[0072]

[0073] Add 500 mL of an aqueous solution containing 0.3 mol of calcium bicarbonate to a four-port reactor, then dropwise add 300 mL of an isopropyl ether solution containing 0.299 mol of 3-methyl-4-yne-1-penten-3-yl calcium, for 60 min After dripping left and right, continue to stir for 30 minutes and then stop the hydrolysis reaction. The temperature of the hydrolysis process is controlled between 30 and 50°C. Centrifuge then to obtain solid calcium carbonate 59.6g. The oil-water mixture was separated to obtain 289 mL of 3-methyl-4-yn-1-penten-3-ol in isopropyl ether and 504 mL of calcium salt solution.

[0074] The isopropyl ether solution of 3-methyl-4-yne-1-penten-3-ol was recovered at 60-80°C under normal pressure, and then rectified to obtain 57.4g of the product, the content of which was detecte...

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Abstract

The invention discloses a process for preparing alcohols by hydrolyzing metal-organic products, which specifically includes the steps of: 1) carrying out a hydrolysis reaction with a solution containing metal-organic products and an aqueous bicarbonate solution to obtain a hydrolyzed solid-liquid mixture; 2) combining step 1 ) The obtained hydrolyzed solid-liquid mixture is subjected to solid-liquid separation to obtain carbonate solid and oil-water mixture respectively; 3) The oil-water mixture described in step 2) is layered to obtain alcohol product solution and water layer; 4) Step 3) described The alcohol product solution is recovered to obtain the alcohol product after the solvent is recovered. The process can realize the effective recycling of waste water, and at the same time, avoid the occurrence of halogenated side reactions in the hydrolysis process, and can effectively improve the product content.

Description

technical field [0001] The invention relates to a post-treatment process for metal organic products, in particular to a process for preparing alcohols by hydrolysis of metal organic products. Background technique [0002] Grignard reagents are an important class of intermediates in organic synthesis with the general formula RMgX. Grignard reagents and various types of ketones, aldehydes, esters and other substances can undergo Grignard reactions to obtain corresponding alcohol metal organic compounds, and then various alcohols can be obtained after acidic hydrolysis. [0003] At present, the hydrolysis method of Grignard reaction to obtain metal organic compounds of alcohols is generally an acidic aqueous solution hydrolysis process. Chinese patent CN 106748943A discloses a method and device for continuous hydrolysis and neutralization of a vitamin A intermediate double Grignard condensate, that is, acid water and an ether solution of a vitamin A intermediate double Grignar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/09C07C33/14C07C33/025C07C33/048
CPCC07C29/09C07C2601/16C07C33/14C07C33/025C07C33/048
Inventor 吕国锋郑兆祥田金金王徐斌汤先亮段晨彬刘丽丽
Owner SHANGYU NHU BIOCHEM IND
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