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Preparation method of cyclic chlorinated phosphate

A chlorophosphate and cyclic technology, which is applied in the field of preparation of cyclic chlorophosphate, can solve the problems of many side reactions, low yield and high risk, and achieve fewer reaction steps, high yield and high selectivity Good results

Active Publication Date: 2021-01-15
JIANGSU GUOTAI SUPER POWER NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method still has following deficiencies: 1, need to use two-step method to synthesize target product, first step reaction produces byproducts such as a large amount of hydrochloric acid, side reaction is many and yield is low, second step reaction is oxidation reaction, reaction process Oxidants need to be oxidized in the process, and the oxidation reaction is a high-risk process with high risk and low yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Synthesis of 2-chloro-2-oxo-1,3,2-dioxaphospholane (COP)

[0033] In the reaction reflux water separator, the inert solvent toluene (900 g) and phosphorus oxychloride (153.0 g, 1.0 mol) were sequentially added under stirring state, and the temperature was raised to 60° C. after mixing uniformly. Then evenly add 1,2 bis(trimethylsiloxy)ethane (195.7g, 0.95mol) dropwise, and the dropwise addition time is 4 hours. The component received from the reflux water separator in the reaction process is trimethylchlorosilane). When the heat preservation reaction time is reached and no gas is generated, stop the reaction immediately and protect the reaction solution with nitrogen. After the above reaction solution was lowered to normal temperature, it was transferred to a rectification device for rectification, and the rectification conditions were controlled at 90°C and 200Pa to obtain 2-chloro-2-oxo-1,3,2-dioxaphospholane (COP ) Crude product 127.5g (0.898mol), yield is 94.5%wt....

Embodiment 2

[0041] Synthesis of 2-chloro-2-oxo-1,3,2-dioxaphospholane (COP)

[0042]In the reaction reflux water separator, the inert solvent acetonitrile (900 g) and phosphorus oxychloride (153.0 g, 1.0 mol) were successively added under stirring state, and the temperature was raised to 60° C. after mixing uniformly. Then, 1,2 bis(trimethylsiloxy)ethane (216.3g, 1.05mol) was added dropwise evenly, and the dropwise addition time was 4 hours. The component received from the reflux water separator in the reaction process is trimethylchlorosilane). When the heat preservation reaction time is reached and no gas is generated, stop the reaction immediately and protect the reaction solution with nitrogen. After the above reaction solution was lowered to normal temperature, it was transferred to a rectification device for rectification, and the rectification conditions were controlled at 90°C and 200Pa to obtain 2-chloro-2-oxo-1,3,2-dioxaphospholane (COP ) crude product 125.2g (0.879mol), yield...

Embodiment 3

[0050] Synthesis of 2-chloro-2-oxo-1,3,2-dioxaphosphorinane

[0051] In the reaction reflux water separator, the inert solvent toluene (900g) and phosphorus oxychloride (153.0g, 1.0mol) were successively added under stirring, and the temperature was raised to 60°C after mixing uniformly. Then evenly add 1,3 bis(trimethylsiloxy)propane (209g, 0.95mol) dropwise for 5 hours. The component received from the reflux water separation device is trimethylchlorosilane). When the heat preservation reaction time is reached and no gas is generated, stop the reaction immediately and protect the reaction solution with nitrogen. After the above reaction solution was lowered to normal temperature, it was transferred to a rectification device for rectification. The rectification conditions were controlled at 90°C and 200Pa to obtain 2-chloro-2-oxo-1,3,2-dioxaphosphorinane crude product 106.4 g (0.680mol), the yield is 71.6%wt. Then transfer the crude 2-chloro-2-oxo-1,3,2-dioxaphosphorinane t...

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Abstract

The present invention relates to a cyclic chlorinated phosphate preparation method, wherein phosphorus oxychloride and alkyl siloxane are subjected to a cyclization reaction in the presence of an aprotic solvent to prepare cyclic chlorinated phosphate, the structural formula of alkyl siloxane is shown in the specification, the structural formula of the cyclic chlorinated phosphate is shown in thespecification, and n is a number between 1 and 5. According to the invention, synthesis is a one-step reaction, the reaction avoids an oxidation reaction (the oxidation reaction is a high-risk process), and the method is high in reaction selectivity and yield, few in reaction steps and suitable for industrial production.

Description

technical field [0001] The invention specifically relates to a preparation method of cyclic chlorophosphate. Background technique [0002] As an important building block of biomedical materials, phosphorus-based heavy metal complex catalysts, stereospecific reaction reagents, and new high-performance flame retardant materials, cyclic chlorophosphates play an important role in new functional materials. For example, in the field of biomedical materials, phosphorylcholine derivatives are synthesized by cyclic chlorophosphoryl ester 2-chloro-2-oxo-1,3,2-dioxaphospholane (COP), which is used for the preparation of drugs. Delivery and release; In the field of new high-performance flame retardant materials, 2-chloro-2-oxo-1,3,2-dioxaphospholane (COP) was used as raw material to synthesize phosphonopropyl phosphate flame retardant Fuel. [0003] In order to prepare cyclic chlorophosphates, Sahar Noori et al [J Solution Chem (2015) 44:1292-1309] proposed in 2015 to use phosphorus o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574
CPCC07F9/65742
Inventor 邹凯顾新红汤涛季宇轩李建中
Owner JIANGSU GUOTAI SUPER POWER NEW MATERIALS