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Allyl amyl glycolate preparation method

A compound, the technology of chloroacetic acid, applied in the field of preparation of glycopyrrolate, can solve the problems of high hazard, high production cost, and difficult quality control, etc., and achieve the effect of reducing hazard, production cost and solid waste

Inactive Publication Date: 2018-10-23
盐城恰爱娜生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the quality control of Gepong ester produced by the currently disclosed method is very difficult, the production cost is too high, and the potential harm is very high.

Method used

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  • Allyl amyl glycolate preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The preparation of embodiment 1 compound II

[0032]

[0033] In a three-necked flask equipped with a stirring bar, add 120ml of N,N-dimethylformamide, add 8.6g of sodium hydroxide, then add 16.4g of chloroacetic acid and 18.6g of allyl chloride, and react at room temperature for 3~4h, After the reaction was completed, part of the DMF was removed by rotary evaporation, then diluted with water, extracted with dichloromethane, the organic layers were combined and concentrated to obtain 20.8 g of compound II, with a yield of 89%.

Embodiment 2

[0034] Preparation of Example 2 Compound I (Gaponate)

[0035]

[0036] Add 185g of isoamyl alcohol and 12.6g of sodium hydroxide into a three-necked flask equipped with a stirring bar and a thermometer, heat to 130~140°C for reflux dehydration for 4 hours, then cool to room temperature, slowly add 18.2g of compound II, and distill and recover isoamyl alcohol after the reaction is complete. Amyl alcohol, then acidified with dilute hydrochloric acid to pH = 6~7, separated the organic layer, and distilled to obtain 22.9 g of colorless and transparent liquid Gelponate, with a yield of 91%. HPLC: 99.5%.

Embodiment 3

[0037] Example 3 Preparation of Compound II

[0038]

[0039] In a three-neck flask equipped with a stirring bar, add 110ml of N,N-dimethylformamide, add 6.0g of sodium hydroxide, then add 14.2g of chloroacetic acid and 11.5g of allyl chloride, and react at room temperature for 3~4h, After the reaction was completed, part of the DMF was removed by rotary evaporation, then diluted with water, extracted with dichloromethane, the organic layers were combined and concentrated to obtain 16.2 g of Compound II, with a yield of 80.3%.

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Abstract

The invention provides an allyl amyl glycolate preparation method, wherein specifically a reaction is performed by replacing the conventional allyl alcohol with vinyl chloride to prepare allyl amyl glycolate. According to the present invention, the method has advantages of simple operation, high yield, high purity, greatly reduced production cost, reduced waste generation and reduced environmentalhazard, wherein the excess vinyl chloride residue in the final product cannot be generated.

Description

technical field [0001] The invention relates to the field of perfume synthesis, in particular to a preparation method of glycopyrrolate. Background technique [0002] Gepong ester, whose structure is shown in formula I, is also known as allyl amyl amyloxyacetate. It is an important synthetic fragrance with strong Gepong aroma and fruity aroma. It is widely used in perfumes, cosmetics, soaps, air Fragrance of various products such as fresheners and detergents. [0003] Zhang Jing'an disclosed the following preparation method of glycopyrrolate in "Catalyzed Synthesis of Allyl Isopentoxy Acetate" (Perfume, Fragrance and Cosmetics, 1995, (4): 31-33): First, react with metal sodium and isoamyl alcohol Sodium isoamyloxide is prepared, and reacted with chloroacetic acid to remove sodium chloride to synthesize isopentyloxyacetic acid; isopentyloxyacetic acid and allyl alcohol are esterified under acid catalysis to prepare gabung ester. Since metal sodium requires absolute anhydrou...

Claims

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Application Information

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IPC IPC(8): C07C67/31C07C69/708
CPCC07C67/11C07C67/31C07C69/708C07C69/63
Inventor 杨正权孙学虎徐安佗
Owner 盐城恰爱娜生物科技有限公司
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