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Synthesis method of polyketone ligand

A synthesis method and ligand technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as handling difficulties and increase production costs, and achieve simple equipment and safe industry. Chemical, high product yield effect

Pending Publication Date: 2022-03-01
CHAMBROAD CHEM IND RES INST CO LTD
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Problems solved by technology

[0004] In above two kinds of preparation methods, the preparation of bis(2-methoxyphenyl) phosphine oxide just needs two-step reaction, and uses multiple solvents, handles difficulty, and there is potential safety hazard in sodium hydrogen in addition, sodium tert-butoxide introduces Tert-butanol, introducing new three wastes treatment problems or increasing production costs

Method used

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  • Synthesis method of polyketone ligand
  • Synthesis method of polyketone ligand
  • Synthesis method of polyketone ligand

Examples

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preparation example Construction

[0024] The present invention provides a polyketone ligand 3,3-dual-[double-(2-methoxyphenyl) phosphine methyl] -1,5-dioxane-snail [5, 5] extol Synthetic method, including the following steps:

[0025] a) Reaction the benzoatoxyl ether to the phosphite in the solvent to give a bis (2-methoxyphenyl) phosphine oxide;

[0026] b) The dual (2-methoxyphenyl) phosphine oxide obtained by step a) is reduced in a solvent to obtain a bis (2-methoxyphenyl) phosphine;

[0027] c) Different (2-methoxyphenyl) phosphine obtained by step b) under the action of the base, in the solvent and 5,5-bis (bromomethyl) -1,5-dioxane-snail [5, 5] Elementalk reaction to obtain polyketone ligand 3,3-dual-[double-(2-methoxyphenyl) phosphine methyl] -1,5-dioxane-snail [5, 5] Elementane.

[0028] The present invention first reacts benzoatoxyl ether to phosphite in a solvent to obtain a bis (2-methoxyphenyl) phosphine oxide. In the present invention, the solvent is preferably tetrahydrofuran and / or diethyl ether...

Embodiment 1

[0067] Method for synthesis of polyketone ligand 3,3-dual-[double-(2-methoxyphenyl) phosphine methyl] -1,5-dioxane [5,5] udeolicane, The specific steps are:

[0068] (1) Preparation of bis (2-methoxyphenyl) phosphine oxide:

[0069] Under anhydrous aerobic conditions, 2.70 g of the benzoyl ether was added to 2.90 ml of tetrahydrofuran, cooled to -20 ° C, start holding the temperature drop of 15.62 ml N-Buli, after the drop is added. Toning temperature was stirred for 1 h, warmed to 30 ° C for 4 h, followed by the tracking detection reaction, cooled to -20 ° C, start controlling the temperature drop of diaphragite 1.38 g, after the dropping, after 1 h, then heated to 30 ° C After the tracking detection reaction is completed, the reaction solution slowly dripped in ice water with 10% hydrochloric acid, and the pH is adjusted to be filled with water. To give a double (2-methoxyphenyl) phosphine oxide of 2.50 g, purity 98.65%, yield 94.13%.

[0070] (2) Preparation of bis (2-methoxyph...

Embodiment 2

[0075] Method for synthesis of polyketone ligand 3,3-dual-[double-(2-methoxyphenyl) phosphine methyl] -1,5-dioxane [5,5] udeolicane, The specific steps are:

[0076] (1) Preparation of bis (2-methoxyphenyl) phosphine oxide:

[0077] Under anhydrous aerobic conditions, the benzo ether 2.81 g and tetramethylenediamine was added to 20 ml of diethyl ether, cooled to -40 ° C, start holding the temperature drop plus 16.25 ml N-Buli solution, after the drop is added Toning temperature was stirred for 1 h, warmed to 40 ° C for 4 h, followed by the test reaction, cooled to -40 ° C, start controlling diethyl phosphite 1.38 g of phosphite, after the dropping, after 2 h, heated to 40 ° C After the tracking detection reaction is completed, the reaction solution slowly dripped in ice water with 10% hydrochloric acid, and the pH is adjusted to be filled with water. To give a double (2-methoxyphenyl) phosphine oxide of 2.55 g, purity 99.21%, yield 96.60%.

[0078] (2) Preparation of bis (2-methox...

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Abstract

The invention provides a synthesis method of a polyketone ligand 3, 3-bis-[bis-(2-methoxyphenyl) phosphinomethyl]-1, 5-dioxa-spiro [5, 5] undecane, which comprises the following steps: a) carrying out reaction on anisole and diethyl phosphite in a solvent to obtain bis (2-methoxyphenyl) phosphine oxide; b) carrying out reduction reaction on the bis (2-methoxyphenyl) phosphine oxide obtained in the step a) in a solvent to obtain bis (2-methoxyphenyl) phosphine hydrogen; and c) reacting the bis (2-methoxyphenyl) phosphine hydrogen obtained in the step b) with 5, 5-bis (bromomethyl)-1, 5-dioxa-spiro [5, 5] undecane in a solvent under the action of alkali to obtain the polyketone ligand 3, 3-bis-[bis-(2-methoxyphenyl) phosphine methyl]-1, 5-dioxa-spiro [5, 5] undecane. Compared with the prior art, specific raw materials are selected to synthesize the polyketone ligand according to specific process steps, the reaction route is simple, needed equipment is simple, energy consumption is low, overall good interaction can be achieved, the product yield is high, quality is good, and the method is safe and easy to industrialize.

Description

Technical field [0001] The present invention relates to the field of fine chemical technology, and more particularly, it is to relate to a polyketone ligand 3, 3-dual-[double-(2-methoxyphenyl) phosphine methyl] -1,5-dioxide Hybrid - Social Synthesis Method of Ultramethane. Background technique [0002] Polyketone (POK) is composed of carbon monoxide, olefin (ethylene, propylene, styrene), polyketone has photodegradation and biodegradable characteristics, and can be further chemically modified, excellent and broadly performed. It becomes a "natural" thermoplastic engineering plastic. During the preparation of polyketone, the polymerization catalyst is typically composed of a system of Pd (II) / bisphosphine ligand / acid, and the catalytic active bisphoscent ligand such as 1,3-double [double (2-methoxy) Baxyl) phosphine group] propane, ((2,2-dimethyl-1,3-dioxidal ring-5,5-di) double (methylene)) double (double (2-methoxy) Baxyl) phosphine), 3,3-dual-[double-(2-methoxyphenyl) phosp...

Claims

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Application Information

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IPC IPC(8): C07F9/655
CPCC07F9/65522
Inventor 王朋朋裴立军高秀云王瑞静曹丽艳张朋朋刘英贤
Owner CHAMBROAD CHEM IND RES INST CO LTD
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