A kind of synthetic technique of tridemorpholine

A synthesis process, the technology of tridecamorpholine, applied in organic chemistry and other directions, can solve the problem of many by-products, and achieve the effects of reducing corrosion intensity, mild reaction conditions, and reducing energy consumption

Active Publication Date: 2019-07-26
江苏富比亚化学品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This reaction process has many by-products and produces a large amount of solid waste, including sodium sulfite, sodium chloride, etc.

Method used

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  • A kind of synthetic technique of tridemorpholine
  • A kind of synthetic technique of tridemorpholine
  • A kind of synthetic technique of tridemorpholine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] 500g tridecyl alcohol, 500g tridecane are added in the reactor;

[0066] Add 10g of catalysts (mixed by methyl copper, binuclear methyl nickel, dimethyl zinc and trimethyl aluminum in a weight ratio of 1:1:1:1) in the reactor, mix under stirring, Introduce hydrogen gas at a rate of 0.1L, and raise the temperature of the reactor to 230°C in about 2 hours;

[0067] When the temperature of the reactor rises to 230°C, start to slowly add 400g of 2,6-dimethylmorpholine dropwise, maintain the pressure in the reactor at 0.3Mpa, and the temperature at 230-240°C until the end of the reaction. Or intermittently water and unreacted 2,6-dimethylmorpholine are taken out from the top of the tower; during the reaction, the reaction sample is detected by GC, such as figure 1 As shown, peaks appear at retention times (min.) of 1.716, 1.838, 1.891, 2.014, 2.273, 2.357, 2.447, 2.530, 4.563, 9.237, 13.301, 13.379, wherein 1.716, 4.563, 9.237 correspond to 2,6 - Dimethylmorpholine (8.299%...

Embodiment 2

[0071] 500g tridecyl alcohol, 400g tridecane are added in the reactor;

[0072] Add 9g of the fresh catalyst used in Example 1 and 2g of the catalyst recovered from Example 1 in the reactor, mix under stirring, feed hydrogen, and heat up the reactor;

[0073] When the temperature of the reaction kettle rose to 225°C, slowly drop 400g of 2,6-dimethylmorpholine and 50g of 2,6-dimethylmorpholine recovered and purified by distillation in Example 1, and keep the reaction kettle The pressure is 0.35Mpa, and the temperature is 230-245°C until the end of the reaction; during the reaction, the reaction sample is detected by GC, such as image 3 As shown, peaks appear at the retention times (min.) of 1.717, 1.840, 1.891, 2.013, 2.061, 2.343, 2.444, 2.576, 2.767, 4.545, 6.983, 7.147, 7.261, 9.238, 13.272, wherein 1.717, 4.545, 9.238 corresponds to 2,6-dimethylmorpholine (7.414%), tridecane+tridecyl alcohol (45.986%), and tridecylmorpholine (45.947%), respectively.

[0074] After the dr...

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PUM

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Abstract

The invention relates to a tridemorph synthesis process which includes the steps: adding tridecyl alcohol and optional solvents into a reaction kettle, adding a catalyst, stirring and mixing mixture,leading into hydrogen, and heating the reaction kettle; adding 2, 6-thebaine when the temperature of the reaction kettle reaches the temperature of 200 DEG C or more, and maintaining the reaction kettle to perform reaction in a certain pressure and at a certain temperature until reaction is completed; post-processing a reactant to obtain a reactant finished product. According to the tridemorph synthesis process, the tridemorph with the purity larger than 99% is acquired under the conditions of high selectivity and high yield, and waste water, waste gas and industrial residues are greatly reduced.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a synthesis process of tridemorpholine. Background technique [0002] Tridemorpholine (Kleopsis), the chemical name is 2,6-dimethyl-4-tridecylmorpholine, also known as N-tridecyl-2,6-dimethylmorpholine. The second morpholine fungicide developed by BASF in 1965 and launched in 1969. The action mechanism and characteristics of tridemorpholine are mainly to inhibit the biosynthesis of ergosterol of pathogenic bacteria. effective against a variety of plant diseases. It can effectively control wheat and barley powdery mildew, leaf rust and stripe rust, cucumber, potato, pea powdery mildew, rubber tree powdery mildew, banana leaf spot. [0003] Tridemorph can be absorbed into the plant through the roots, stems and leaves of the plant, and move upward in the xylem, but only slightly transferred in the phloem. Can maintain a long duration. [0004] As a fungicide, tridemorpholine can g...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D265/30
CPCC07D265/30
Inventor 吴邦元施仲锋李焕成王福龙杨钦
Owner 江苏富比亚化学品有限公司
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