Method for preparing ammonium salts of cyclohexanpentol phosphate ester

A technology of ammonium cyclohexapentyl phosphate and cyclohexapentyl phosphate, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of polyol phosphate Ammonium salt report, no preparation method and report of cyclohexapentyl phosphate ammonium salt, achieve the effects of low pollution, common and easy-to-obtain raw materials, and simple preparation method

Inactive Publication Date: 2006-09-13
SICHUAN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] But there is no report about polyol phosphate ammonium salt at present, more there is no report about cyclohexapentyl phosphate ammonium salt and preparation method thereof etc.

Method used

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  • Method for preparing ammonium salts of cyclohexanpentol phosphate ester
  • Method for preparing ammonium salts of cyclohexanpentol phosphate ester

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0024] Prepare cyclohexapentyl phosphate N-hydroxysucciniminium salt by the method of this embodiment, comprising the following steps:

[0025] (1) Synthesis of cyclohexanepentaol: add about 6g of glucose, 2ml of methanol, and 20ml of THF into a three-necked flask; add 2ml of concentrated sulfuric acid dropwise under stirring, continue stirring for about 4 hours after dropping, and adjust the reaction mixture with 40% NaOH aqueous solution pH value to 9-10, filter off the precipitated white solid, distill off THF; use CHCl 3 Extract 3 times, each time with CHCl 3 About 80ml, combine the extracts, add appropriate amount of K 2 CO 3 to dry; then distill off CHCl 3 , the residue was separated by silica gel column chromatography, and CHCl 3 As a eluting agent, the obtained eluent is desolvated to obtain a viscous substance, namely methyl glucoside. Add 30mlDMF to methyl glucoside, use appropriate amount of CsF and triethylphenyl ammonium chloride as catalyst, realize phase tr...

Embodiment 2

[0029] Prepare tricyclohexapentyl phosphate N-hydroxysucciniminium salt by the method of this embodiment, comprising the following steps:

[0030] (1) Synthesis of cyclohexanepentol: Add 5.72g of glucose, 2ml of methanol, and 20ml of THF into a three-necked flask; add 2ml of concentrated sulfuric acid dropwise under stirring, continue stirring for about 3h after dropping, and adjust the reaction mixture with 40% NaOH aqueous solution pH value to 9-10, filter off the precipitated white solid, distill off THF; use CHCl 3 Extract 3 times, each time with CHCl 3 About 70ml, combine the extracts, add appropriate amount of K 2 CO 3 to dry; then distill off CHCl 3 , the residue was separated by silica gel column chromatography, and CHCl 3 As a eluting agent, the obtained eluent is desolvated to obtain a viscous substance, namely methyl glucoside. Add 30ml DMF to methyl glucoside, use appropriate amount of CsF and triethylphenylammonium chloride as catalyst to realize phase transfer...

Embodiment 3

[0034] Prepare diisopropylammonium cyclohexapentyl phosphate by the method of this embodiment, comprising the following steps:

[0035] (1), synthesis of cyclohexanepentaol: add 5g glucose, 2ml methanol, and 20ml THF to a three-necked flask; add 2ml concentrated sulfuric acid dropwise under stirring, continue stirring for about 3h after dropping, adjust the reaction mixture with 40% NaOH aqueous solution pH value to 9 ~ 10, filter off the precipitated white solid, distill off THF; use CHCl 3 Extract 2 times, each time with CHCl 3 About 70ml, add appropriate amount of K 2 CO 3 to dry; then distill off CHCl 3 , the residue was separated by silica gel column chromatography, and CHCl 3 As a eluting agent, the obtained eluent is desolvated to obtain a viscous substance, namely methyl glucoside. Add 30ml of DMF to methyl glucoside, and use appropriate amount of CsF and triethylphenyl ammonium chloride as catalyst to realize phase transfer catalysis, and obtain the intermediate ...

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Abstract

The invention relates to producing method of the viburnitol phosphate ester ammouium salt, which is the compound expressed by the general equation. The R1 is elected from the amine having the atomicity of 3-18; the R2 and R3 are elected form -H-PO (OH) 2, or PO (OH)'2R, R' is also elected from the amine having the atomicity of 3-18. The producing method of the compound includes the composing the viburnitor, the viburnitol phosphate ester, and the viburnitol phosphate ester ammouium salt. The method has some merits of the simplicity of operation,the cheap cost and the low environmental pollution.

Description

technical field [0001] The invention relates to a preparation method of a cyclopolyol phosphate ammonium salt compound. Background technique [0002] Polyol phosphate esters are a class of widely used compounds, which can be used as flame retardants, water treatment agents, surfactants, etc. It is mainly used in circulating water cooling systems such as oil refineries, chemical plants, chemical fertilizer plants, steel plants, air conditioning systems and copper heat exchangers, as a scale and corrosion inhibitor for water treatment, especially suitable for process materials with serious leakage and corrosion Scale and corrosion inhibitors for circulating water systems and oilfield water injection. [0003] In addition, polyol phosphates and amines are excellent buffers for metals such as copper, tin, aluminum and aluminum alloys, zinc, and steel in aqueous solutions. The polyol phosphates synthesized from sugars have a molecular structure similar to natural phospholipids,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/117
Inventor 赵仕林易灵李可廖洋
Owner SICHUAN NORMAL UNIVERSITY
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