3-methylamine tetrahydrofuran preparation method

A technology of methylamine tetrahydrofuran and tetrahydrofuran formaldehyde, which is applied in the field of preparation of 3-methylamine tetrahydrofuran, can solve the problems of not being suitable for industrial production and explosion risk, and achieve the effects of short reaction steps, less pollution of three wastes, and lower production costs

Active Publication Date: 2017-02-15
浙江捷达科技有限公司
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Problems solved by technology

If the raw material sodium azide used in this reaction is improperly handled, there is a risk of explosion, and it is not suitable for industrial production.

Method used

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  • 3-methylamine tetrahydrofuran preparation method
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  • 3-methylamine tetrahydrofuran preparation method

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Experimental program
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Effect test

Embodiment 1

[0027] The preparation of embodiment 1 3-methylamine tetrahydrofuran

[0028] (1) Cyclization reaction to prepare 2,5-dihydrofuran

[0029] Weigh 1000kg 1,4-butenediol for use. Add 30kg of alumina and 100kg of 1,4-butenediol to the reaction kettle successively, stir and mix evenly, then raise the temperature to 130°C, then continue to add 900kg of 1,4-butenediol dropwise until the reaction is completed, and keep the temperature for 8 hours During the reaction process, the fraction below 102°C was continuously distilled, and the obtained fraction was left to stand for stratification. After the organic layer was dried and dehydrated, it was rectified at atmospheric pressure to collect the fraction at 64-67°C; the fraction at 64-67°C was collected in the water layer through distillation The desired 2,5-dihydrofuran was obtained by mixing the fractions at 64-67°C obtained twice, and a total of 787.5 kg of 2,5-dihydrofuran was obtained, with an HPLC purity of 95.03% and a yield of...

Embodiment 2-3

[0034] Example 2-3 Ring closure reaction to prepare 2,5-dihydrofuran

[0035] 2,5-dihydrofuran was prepared using the same operating method and the same type of raw materials as in step (1) of Example 1, the difference being the feed ratio and reaction time. The experimental results obtained are shown in Table 1:

[0036] Table 1:

[0037]

Embodiment 4-5

[0038] Embodiment 4-5 Formylation reaction prepares 3-THF

[0039] Adopt the operation method identical with embodiment 1 step (2) and same raw material to prepare 3-tetrahydrofurfuran formaldehyde, difference is feed ratio, water gas pressure, reaction temperature and reaction time, gained experimental result is as shown in table 2:

[0040] Table 2:

[0041]

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Abstract

The invention provides a 3-methylamine tetrahydrofuran preparation method, wherein 1,4-butenediol is adopted as a raw material and is subjected to cyclization dehydration under the catalysis effect of a solid acid to produce 2,5-dihydrofuran, the 2,5-dihydrofuran reacts with water gas under the catalysis effect of cobalt acetate to produce 3-tetrahydrofuran formaldehyde, and the 3-tetrahydrofuran formaldehyde, ammonia gas and hydrogen gas are subjected to a hydrogenation reaction under the catalysis effect of 5% Pd/C to prepare the target product3-methylamine tetrahydrofuran, wherein the purity is 98.12%, and the total yield is 74.16%. According to the present invention, the preparation method has advantages of cheap and easily available raw materials, less steps, simple operation, high product purity, high yield, less three-waste pollution and production cost reducing, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of 3-methylamine tetrahydrofuran, which belongs to the technical field of organic synthesis. Background technique [0002] Dinotefuran is a neonicotinoid insecticide developed by Mitsui East Asia Chemical Co., Ltd., which is quite different from the existing neonicotinoid insecticides in chemical structure. It replaces the previous chloropyridyl with tetrahydrofuryl , Chlorothiazolyl, free of halogen elements. At the same time, it is also different from nicotine in terms of performance. It is very safe for mammals. Its acute oral LD50 is 2450mg / kg for male rats and 2275mg / kg for female rats; 2840mg / kg for male mice and 2275mg / kg for female mice. 2000mg / kg. For rats, the acute percutaneous LD50>2000mg / kg (female and male), has no teratogenicity, carcinogenicity and mutagenicity. Dinotefuran is also very safe to aquatic organisms. The fish toxicity test shows that dinotefuran has a nm(48h)>1000mg / L t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/14
CPCC07D307/14
Inventor 陶贤鉴孙荣根
Owner 浙江捷达科技有限公司
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