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Method for synthesizing 1-(1, 4-dioxaspiro [4, 5] decane-8-yl) ethanone

A technology of dioxaspiro and decane, which is applied in the field of 1-ethanone synthesis, can solve the problems of high product cost, unfavorable preparation and use, and difficult preparation of precursor carboxylic acid, and achieve high yield and mild reaction conditions Effect

Pending Publication Date: 2021-08-17
NANJING ACCELEDEV TECH DEV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0002] Traditional literature and practice adopt weinreb amide method to prepare more when preparing 1-(1,4-dioxaspiro[4,5]decane-8-yl)ethanone, but the precursor carboxylic acid of this compound is relatively Difficult to make, resulting in high cost of the product, which is not conducive to the preparation and use of large quantities

Method used

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  • Method for synthesizing 1-(1, 4-dioxaspiro [4, 5] decane-8-yl) ethanone
  • Method for synthesizing 1-(1, 4-dioxaspiro [4, 5] decane-8-yl) ethanone
  • Method for synthesizing 1-(1, 4-dioxaspiro [4, 5] decane-8-yl) ethanone

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Embodiment

[0029] refer to figure 1 , a method for synthesizing 1-(1,4-dioxaspiro[4,5]decane-8-yl)ethanone, the technical route is:

[0030]

[0031] It includes the following steps:

[0032] S1, add tetrahydrofuran to the 500ml single-necked bottle;

[0033] S2. Adding an ether solution of methylmagnesium iodide at a temperature of -10°C to 0°C;

[0034] S3. Adding a THF solution of 1,4-dioxaspiro[4,5]decane-8-carbonitrile at a temperature of 0°C to 5°C;

[0035] S4. Stir at 0°C to 5°C for 12-24 hours, gas phase detection of raw materials <5%, and quench with saturated ammonium chloride solution;

[0036] S5. Extract with ethyl acetate, add saturated sodium bisulfite solution, and stir at a temperature of 15° C. to 30° C. for 30 minutes;

[0037] S6, liquid separation, extraction with ethyl acetate, abandoning the organic phase;

[0038] S7, adjusting the pH of the aqueous phase to 8-9 with sodium hydroxide solution, and extracting with ethyl acetate;

[0039] S8. The solvent w...

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Abstract

The invention belongs to the technical field of synthesis of 1-(1, 4-dioxaspiro [4, 5] decane-8-yl) ethanone, and particularly relates to a method for synthesizing 1-(1, 4-dioxaspiro [4, 5] decane-8-yl) ethanone, which comprises the following steps: adding tetrahydrofuran into a 500ml single-mouth bottle; adding an diethyl ether solution of methyl magnesium iodide at the temperature of-10 DEG C to 0 DEG C; adding a tetrahydrofuran solution of 1, 4-dioxaspiro [4, 5] decane-8-formonitrile at the temperature of 0 DEG C to 5 DEG C; stirring for 12-24 hours at the temperature of 0-5 DEG C, and quenching by using a saturated ammonium chloride solution when the gas phase detection raw material is less than 5%; extracting with ethyl acetate, adding a saturated sodium hydrogen sulfite solution, and stirring for 30 minutes at the temperature of 15-30 DEG C; separating liquid, and extracting with ethyl acetate; adjusting the pH value of the water phase to 8-9 by using a sodium hydroxide solution, and extracting by using ethyl acetate; and performing reduced pressure distillation at 40-50 DEG C to remove the solvent. The invention develops a new path which is obtained by one-step reaction of a precursor which is relatively easy to prepare, the reaction condition is mild, and the yield is relatively high.

Description

technical field [0001] The present invention relates to the technical field of 1-(1,4-dioxaspiro[4,5]decane-8-yl)ethanone synthesis, in particular to a method for synthesizing 1-(1,4-dioxaspiro[4,5] ,5] the method of decan-8-yl)ethanone. Background technique [0002] Traditional literature and practice adopt weinreb amide method to prepare more when preparing 1-(1,4-dioxaspiro[4,5]decane-8-yl)ethanone, but the precursor carboxylic acid of this compound is relatively It is difficult to make, which leads to high cost of the product, which is not conducive to the preparation and use of large quantities. [0003] Therefore, we propose a method to synthesize 1-(1,4-dioxaspiro[4,5]decane-8-yl)ethanone to solve the above problems. Contents of the invention [0004] The purpose of the present invention is to solve the shortcomings in the prior art, and propose a method for synthesizing 1-(1,4-dioxaspiro[4,5]decane-8-yl)ethanone. [0005] In order to achieve the above object, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/72
CPCC07D317/72
Inventor 成杨蔡晟
Owner NANJING ACCELEDEV TECH DEV