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Preparation method of 3-morpholone

A technology of morpholinone and ethanolamine, applied in the field of preparation of 3-morpholinone, can solve the problems of many by-products, low yield, low industrialization value, etc., and achieves low cost, low content of by-products, and easy-to-obtain raw materials Effect

Inactive Publication Date: 2010-06-16
SUZHOU TIANMA SPECIALTY CHEM
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Problems solved by technology

[0004] The first method has low yield, many by-products, and little industrial value
The second method also has low yield and many by-products, and it is prepared by column chromatography, which has little industrial value

Method used

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  • Preparation method of 3-morpholone
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preparation example Construction

[0017] The preparation method of 3-morpholinone, such as figure 1 As shown, first nitrogen protection, under the action of alkali or mixed alkali, cool ethanolamine and organic solvent or mixed solvent to 0~-10°C, add ethyl chloride dropwise, and control the temperature at 0~-6°C, Then heat up to 30-80°C and stir for 0.2-2 hours, filter, wash the solid with solvent, combine the mother liquor, evaporate the solvent, and recrystallize to obtain pure 3-morpholinone.

[0018] Among them, the alkali is one of sodium metal, sodium hydride, potassium tert-butoxide, sodium tert-butoxide, and sodium isopropoxide, and the mixed alkali is sodium metal, sodium hydride, potassium tert-butoxide, sodium tert-butoxide, and isopropoxide. A mixture of several types of sodium alkoxide. The organic solvent is one of toluene, isopropanol, tert-butanol, ethanol, and methanol, and the mixed solvent is a mixed solvent of several kinds of toluene, isopropanol, tert-butanol, ethanol, and methanol. Th...

Embodiment 1

[0020] Under nitrogen protection, add 11.5g of metallic sodium in batches to a solution containing 30.5g of ethanolamine and 500ml of isopropanol, raise the temperature to 50°C, stir until the sodium dissolves, cool the reaction solution to 0~-10°C, and add dropwise 55.2 g of ethyl chloride, temperature controlled at 0~-6°C, then warmed up to 30~80°C and stirred for 0.2~2h, filtered, the solid was washed with a solvent, the mother liquor was combined, the solvent was evaporated, and ethyl acetate and iso Propanol was recrystallized to obtain 34.1 g of pure 3-morpholinone, with a yield of 75% and a GC purity of 99.5%.

[0021] Elemental Analysis: Theoretical: C, 47.52; H, 6.98, N, 13.85, O, 31.65. Found: C, 47.54; H, 6.99, N, 13.83, O, 31.64.

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Abstract

The invention provides a preparation method of 3-morpholone, which comprises the steps of: firstly, under the protection of nitrogen, cooling ethanolamine and organic solvent or a mixed solvent to below 0--10 DEG C under the action of alkali or mixed alkali, dropwise adding ethyl chloroacetate, controlling the temperature below 0--6 DEG C; and secondly, raising the temperature to 30-80 DEG C, stirring for 0.2-2h, filtering, washing solid with a solvent, merging mother solutions, evaporating to remove the solvent, and recrystallizing to obtain the pure product of the 3-morpholone. The preparation method has the characteristics of easy obtaining of raw materials, simple process, low cost, high product purity, low content of side products and the like. The yield of the 3-morpholone is 20-80 percent. The invention is suitable for large-scale industrialized production.

Description

technical field [0001] The invention relates to a preparation method of 3-morpholinone, which belongs to the field of organic synthesis and preparation chemistry. Background technique [0002] 3-Morpholinone is a very important organic intermediate, which is widely used in pharmaceutical chemical industry, polymer chemistry and other fields. [0003] The preparation method of 3-morpholinone mainly contains two kinds: 1. use dioxane as solvent, under the effect of metal sodium, ethanolamine and ethyl chloroacetate prepare 3-morpholinone [Bulletin de la Societe Chimiquede France, 287 -9; 1953]; ②Sodium hydride as base, ethanolamine and ethyl chloroacetate in dioxane to prepare 3-morpholinone [WO 2006055951]. [0004] The first method has low yield, many by-products, and little industrial value. The second method has low yield and many by-products, and is prepared by column chromatography, which has little industrial value. Contents of the invention [0005] The object of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D265/32
Inventor 唐满平罗勇初虹任海峰刘世领
Owner SUZHOU TIANMA SPECIALTY CHEM
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