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Preparation method of N-isotridecyl-2,6-dimethyl morpholine

A technology of dimethylmorpholine and isotridecyl, which is applied in the field of N-isotridecyl-2, can solve the problems of large amount of dilution solvent, high price and high production cost, and achieves low cost and high yield. High, high product purity effect

Inactive Publication Date: 2007-03-07
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this method is that it also uses high-priced raw materials, and it needs to introduce a specific catalyst to make it. The amount of dilution solvent is large, and the separation and recovery of high boiling point dilution solvent after the reaction, as well as the service life of the catalyst, poisoning and other factors all cause production costs. higher reason

Method used

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  • Preparation method of N-isotridecyl-2,6-dimethyl morpholine
  • Preparation method of N-isotridecyl-2,6-dimethyl morpholine

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Add 79 grams of bromoisotridecane, 73 grams of 2,6-dimethylmorpholine, 10 grams of sodium carbonate and 8 grams of potassium carbonate into a three-necked reaction flask, stir and heat to 125°C, and react for 5 hours. Cool the reaction material to 90°C, slowly add 20 grams of 30% sodium hydroxide solution dropwise to basify the material, after the basification is completed, the reaction product is cooled and left to stand, and the lower layer of salt and brine solution is separated, and the upper layer of oil is vacuum distilled 88.5 g of N-isotridecyl-2,6-dimethylmorpholine was obtained, with a yield of 96.7% and a content of 97.5% (HPLC). At the same time, about 37 grams of 2,6-dimethylmorpholine are recovered, with a recovery rate of 95%, which can be directly recycled.

Embodiment 2

[0019] Other conditions are the same as in Example 1, using 66 grams of chloroisotridecane instead of bromoisotridecane, adding 62 grams of 2,6-dimethylmorpholine, and adding 18 grams of sodium hydroxide at the same time, and the reaction temperature is 135 ° C , and the reaction time was 7 hours to obtain 87.8 grams of N-isotridecyl-2,6-dimethylmorpholine, with a yield of 96.0% and a content of 97.6% (HPLC). The recovery rate of 2,6-dimethylmorpholine is about 95%, which can be recycled directly.

Embodiment 3

[0021] Other conditions are the same as Example 1, add 17 grams of 2,6-dimethylmorpholine, 35 grams of 2,6-dimethylmorpholine reclaimed, add 12 grams of sodium hydroxide and 6 grams of potassium bicarbonate simultaneously, react The temperature was 150°C to 160°C, and the reaction time was 4 hours to obtain 89.3 grams of N-isotridecyl-2,6-dimethylmorpholine, with a yield of 97.5% and a content of 97.5% (HPLC), 2,6- The recovery rate of dimethylmorpholine is about 95%, which can be recycled continuously.

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Abstract

The invention discloses a preparing method of N-isotridecanoic-2, 6-dimethyl morpholine, which comprises the following steps: adopting one or random two components of isotridecanoic-2, 6-dimethyl morpholine, hydroxide of alkaline metal or carbonate or bicarbonate as raw material; reacting under 100-160 deg.c for 4-12h; stewing the reacted product; laminating; distilling; separating to obtain the product with receiving rate over 96.0% with 97.5% HPLC; recycling excessive non-reacted 2, 6-dimethyl morpholine.

Description

technical field [0001] The present invention relates to organic heterocyclic bactericide original drug, in particular to a preparation method of N-isotridecyl-2,6-dimethylmorpholine. Background technique [0002] N-isotridecyl-2,6-dimethylmorpholine (tridecylmorpholine for short) is a systemic broad-spectrum heterocyclic fungicide, which is effective against a variety of diseases caused by basidiomycetes, ascomycetes and half-knowledge fungi. Plant diseases have good efficacy, mainly used for the prevention and treatment of wheat, barley powdery mildew, leaf rust, stripe rust, cucumber, pea, potato, rubber tree powdery mildew, tea cake disease and rubber tree red root disease. It is a fungicide with low toxicity and safe use ("Safety Evaluation of Tridemorpholine", Occupation and Health [J], 2005, Vol. 21, No. 6, pp. 803-806), belonging to One of the ideal fungicide varieties to promote and encourage industrialization in our country. [0003] At present, the preparation me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D265/30
Inventor 吕耀宏
Owner ZHEJIANG SCI-TECH UNIV
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