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Synthesis method of tert-butyl-8-oxa-3, 11-diazaspiro [5.6] dodecane-3-formate

A technology of diazaspiro and synthetic method, which is applied in the field of synthesis of tert-butyl-8-oxa-3,11-diazaspiro[5.6]dodecane-3-carboxylate, can solve the problem of Synthetic method and other issues, to achieve the effect of short route and reasonable design

Active Publication Date: 2020-08-25
成都药明康德新药开发有限公司
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Problems solved by technology

Mainly solve the technical problems that there is no synthesis method at present

Method used

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  • Synthesis method of tert-butyl-8-oxa-3, 11-diazaspiro [5.6] dodecane-3-formate
  • Synthesis method of tert-butyl-8-oxa-3, 11-diazaspiro [5.6] dodecane-3-formate

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Embodiment

[0012] Step 1: Dissolve 60 g of compound 1 in 500 mL of anhydrous tetrahydrofuran solution, cool down to 0°C, and slowly add 12 g of sodium hydride powder in batches. The reaction solution was naturally warmed to room temperature, then heated to 66°C, refluxed for 1 hour, and then cooled to 0°C. Dissolve 54 g of ethyl bromoacetate in 200 mL of anhydrous tetrahydrofuran, slowly add it to the previous reaction system, and keep the temperature at 0°C. The reaction solution was warmed to room temperature and stirred for 8 hours. The reaction solution was quenched with water, extracted with ethyl acetate, dried over anhydrous sodium sulfate and filtered, and the filtrate was concentrated under reduced pressure to obtain 98 g of crude compound 2.

[0013] Step 2: 95 g of crude compound 2 and 55 g of Raney nickel were placed in 1 L of ethanol, and stirred for 8 hours at 40° C. under a hydrogen pressure of 50 Psi. The reaction solution was filtered with diatomaceous earth, and the f...

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Abstract

The invention relates to a synthesis method of tert-butyl-8-oxa-3, 11-diazaspiro [5.6] dodecane-3-formate, and mainly solves the technical problem that no suitable industrial synthesis method exists at present. The method comprises the following four steps: 1, reacting a compound 1 with ethyl bromoacetate to obtain a compound 2; 2, adding raney nickel into the compound 2 so as to obtain a compound3 through hydrogenation reduction; 3, cyclizing the compound 3 in ethanol by using sodium ethoxide to obtain a compound 4; and 4, reducing amide of the compound 4 in tetrahydrofuran by using a boranedimethyl sulfide complex to obtain a compound 5, with the reaction formula shown in the descriptions in the invention.

Description

technical field [0001] The invention relates to a synthesis method of compound tert-butyl-8-oxa-3,11-diazaspiro[5.6]dodecane-3-carboxylate. Background technique [0002] Compound tert-butyl-8-oxa-3,11-diazaspiro[5.6]dodecane-3-carboxylate (CAS: 1824005-85-7) and related derivatives in medicinal chemistry and organic synthesis has wide application. Currently, there are few reports on the synthesis of tert-butyl-8-oxa-3,11-diazaspiro[5.6]dodecane-3-carboxylate. 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] The purpose of the present invention is to develop a kind of tert-butyl-8-oxa-3,11-diazaspiro[5.6]dodecane-3 with easy to get raw material, easy to operate, easy to control reaction and high yield. - Synthetic method of formate esters. It mainly solves the technical problem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D498/10
CPCC07D498/10
Inventor 张大为周强高明飞姚宝元兰倩倩赵廷王曦卫维魏昕睿谭汝鹏贾涛白有银孙春付新雨于凌波马汝建
Owner 成都药明康德新药开发有限公司
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