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Synthesis method of 7-hydroxymethyl-2,5-diazaspiro [3,4] octane-2-dimethylethylester

A technology of tert-butyl formate and diazaspiro, which is applied in the synthesis field of 7-hydroxymethyl-2,5-diazaspiro[3,4]octane-2-tert-butyl formate, can solve the problem of There are no problems such as being suitable for industrial synthesis methods, and the effects of reasonable reaction process design, easy reaction and convenient operation are achieved.

Active Publication Date: 2017-11-24
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 problem that there is no suitable industrial synthesis method at present

Method used

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  • Synthesis method of 7-hydroxymethyl-2,5-diazaspiro [3,4] octane-2-dimethylethylester

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Embodiment

[0012] Step 1: Sodium hydride (89.7 g, 2.24 mol, purity: 60%) was dissolved in anhydrous THF (3.5 L), and the THF solution of Compound 1 was added dropwise at 0°C (503 g of Compound 1 was dissolved in 3.5 L of water tetrahydrofuran), reacted at 0 ℃ for 1 hour, the reaction solution changed from cloudy to clear; TLC monitored the completion of the reaction, added 1.2 L saturated ammonium chloride solution, then added 1.2 L ethyl acetate, stirred for 5 minutes, separated the organic phase, water phase was extracted 3 times with ethyl acetate (400mL / time); the organic phase was washed 2 times with saturated brine (500mL / time), dried over anhydrous sodium sulfate, and concentrated to obtain 671g yellow oily crude product (2 batches); the crude product was directly Go to the next reaction.

[0013] Step 2: Dissolve the crude compound 2 (750.0 g, 3.1 mol) and benzylamine (333 g, 3.1 mol) in 6 L of ethanol, react at 80°C for 12 hours under stirring, monitor the completion of the reac...

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Abstract

The invention relates to a synthesis method of a compound of 7-hydroxymethyl-2,5-diazaspiro [3,4] octane-2-dimethylethylester, and mainly solves the technical problem that no industrial method suitable for industrial synthesis exists in the prior art. A compound 1 and triethyl-phosphite are used as raw materials for synthesizing and obtaining the final compound through eight steps. A reaction formula is shown in the specification.

Description

technical field [0001] The invention relates to a synthesis method of compound 7-hydroxymethyl-2,5-diazaspiro[3,4]octane-2-carboxylic acid tert-butyl ester. Background technique [0002] The compound 7-hydroxymethyl-2,5-diazaspiro[3,4]octane-2-carboxylate tert-butyl ester (MDL Number: MFCD28992161&CAS: 1936549-36-8) and related derivatives in medicinal chemistry and Widely used in organic synthesis. Currently, there are few reports on the synthesis methods of tert-butyl 7-hydroxymethyl-2,5-diazaspiro[3,4]octane-2-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 7-hydroxymethyl-2,5-diazaspiro[3,4]octane-2-carboxylic acid that has raw materials easy to get, easy to operate, easy to control and high yield Sy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/10
CPCC07D487/10
Inventor 张大为周强赵红双高明飞于智宇姚宝元卢荣昌白有银孙春刘雨雷韩华欣付新雨卢仔倚李旭东于凌波马汝建
Owner 成都药明康德新药开发有限公司
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