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A kind of synthetic method of (5-fluoropyrimidin-4-yl)methanol

A synthetic method, fluoropyrimidine technology, applied in the field of synthesis of (5-fluoropyrimidin-4-yl)methanol, achieving the effect of reasonable design, short route and simple operation

Active Publication Date: 2022-03-11
阿里生物新材料(常州)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the synthetic method of 5-fluoropyrimidin-4-yl) methanol is rarely reported in the literature

Method used

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Examples

Experimental program
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preparation example Construction

[0025] A synthetic method of (5-fluoropyrimidin-4-yl)methanol, the synthetic method comprises the following reaction formula:

[0026] ;

[0027] Comprising the following synthetic steps:

[0028] (1) According to the mass ratio of compound A, oxidizing agent and acid as 1:1~3:2~4, the solid-liquid ratio g / mL of compound A and methanol is 1:22~28, take the material, compound A, Put oxidizing agent, acid and methanol into the reactor, protect with nitrogen, heat and react to obtain compound B;

[0029] (2) According to the mass ratio of compound B, catalyst and sodium acetate as 4-8:2-3:3-5, and the solid-liquid ratio g / mL of compound B and solvent as 1:50-55, take the material and put Put compound B, catalyst, sodium acetate and solvent into a reaction kettle, increase the pressure, heat, and react to obtain compound C, namely (5-fluoropyrimidin-4-yl)methanol.

Embodiment 1

[0031] The oxidizing agent is dibenzoyl peroxide.

[0032] The acid was trifluoromethanesulfonic acid.

[0033] The catalyst is palladium carbon catalyst.

[0034] The solvent is any one of ethanol, methanol, and propanol.

[0035] A synthetic method of (5-fluoropyrimidin-4-yl)methanol, the synthetic method comprising steps:

[0036] (1) Take 100g of compound A, 220g of oxidant, 100g of acid and 2.5L of methanol into the reactor, use nitrogen to replace 3 times, nitrogen protection, heat to 68°C, react for 18h, TLC detection, the reaction of raw materials is complete, concentrate Reaction solution, methanol and acid were removed, the concentrate was added to 5L ethyl acetate, saturated sodium bicarbonate adjusted the pH to 7, extracted with ethyl acetate, concentrated, and column chromatography gave 45 g of white solid, namely compound B, with a purity of 98.3% ;

[0037] (2) Put 45g of compound B, 20g of catalyst, 30g of sodium acetate and 2L of solvent into an autoclave,...

Embodiment 2

[0040] The oxidizing agent is dibenzoyl peroxide.

[0041] The acid is either acetic acid or methanesulfonic acid.

[0042] The catalyst is palladium carbon catalyst.

[0043] The solvent is any one of ethanol, methanol, and propanol.

[0044] A synthetic method of (5-fluoropyrimidin-4-yl)methanol, the synthetic method comprising steps:

[0045] (1) Take 100g of compound A, 220g of oxidant, 100g of acid and 2.5L of methanol into the reactor, use nitrogen to replace 3 times, nitrogen protection, heat to 68°C, react for 18h, TLC detection, the reaction of raw materials is complete, concentrate Reaction solution, methanol and acid were removed, the concentrate was added to 5L ethyl acetate, saturated sodium bicarbonate adjusted the pH to 7, extracted with ethyl acetate, concentrated, and column chromatography gave 43g of white solid, namely compound B, with a purity of 96.8% ;

[0046] (2) Put 45g of compound B, 20g of catalyst, 30g of sodium acetate and 2L of solvent into an...

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Abstract

The invention belongs to pharmaceutical intermediates, in particular to a method for synthesizing (5-fluoropyrimidin-4-yl)methanol. In the present invention, compound A is used as a starting material, oxidized under the action of an oxidizing agent, and reacted with a catalyst to obtain (5-fluoropyrimidin-4-yl)methanol. The present invention provides a (5-fluoropyrimidine-4-yl)methanol for the first time -4-yl)methanol synthesis method provides a synthetic route for the synthesis of (5-fluoropyrimidin-4-yl)methanol, and the synthetic method is short in route, reasonable in design, simple in operation and easy to control.

Description

technical field [0001] The invention belongs to pharmaceutical intermediates, in particular to a method for synthesizing (5-fluoropyrimidin-4-yl)methanol. Background technique [0002] The synthesis method of the compound 5-fluoropyrimidin-4-yl)methanol and related derivatives are widely used in medicinal chemistry and organic synthesis. At present, the synthesis method of 5-fluoropyrimidin-4-yl)methanol is rarely reported in the literature. Therefore, it is necessary to develop a synthetic method that is easy to obtain raw materials, easy to operate, easy to control the reaction, suitable for overall yield, and suitable for industrial production. Contents of the invention [0003] Technical problem to be solved by the present invention: In view of the above-mentioned problems, provide . [0004] In order to solve the problems of the technologies described above, the present invention adopts the following technical solutions: [0005] A synthetic method of (5-fluoropyri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/30
CPCC07D239/30
Inventor 史建云王超
Owner 阿里生物新材料(常州)有限公司
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