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Method for preparing 3-ammoniac methyl-3-methyl trimethylene oxide

A technology of methyl oxetane and aminomethyl, applied in the field of preparation of 3-aminomethyl-3-methyl oxetane, which can solve the problems of lengthy process, many reaction steps, and tediousness

Inactive Publication Date: 2011-05-11
LIMING RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method has many reaction steps, and the process is lengthy and cumbersome. It needs to use toxic organic solvents such as pyridine, and there are many three wastes.

Method used

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  • Method for preparing 3-ammoniac methyl-3-methyl trimethylene oxide
  • Method for preparing 3-ammoniac methyl-3-methyl trimethylene oxide
  • Method for preparing 3-ammoniac methyl-3-methyl trimethylene oxide

Examples

Experimental program
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Effect test

Embodiment 1

[0022] At room temperature, add 121g CMMO (1mol) to the 1.5L high-pressure ammoniation reactor, high-purity N 2 After sufficient replacement, press 375g of liquid ammonia (22mol) into the reaction kettle with high-purity nitrogen of 0.6-0.70MPa. Heating and stirring, the temperature in the kettle is raised to 80℃~85℃, and the pressure is increased from 0.6MPa to 3.3~3.5MPa. After reacting at this temperature and pressure for 9 hours, the material in the kettle is cooled to room temperature. Lead unreacted excess liquid ammonia into an absorption bottle filled with a sufficient amount of 25% sulfuric acid solution, and empty it after absorption. Then, add 400ml of ethanol to the kettle, stir, and discharge the material. The material is cooled to 0-5°C. A large amount of white crystals of ammonium chloride appear in the solution. Filter and collect the filtrate. Ethanol is removed by evaporation under normal pressure until the solution temperature When the temperature rises to ...

Embodiment 2

[0024] At room temperature, add 121g CMMO (1mol) to the 1.5L high-pressure ammoniation reactor, high-purity N 2 After sufficient replacement, 410 g of liquid ammonia (24 mol) was pressed into the reaction kettle using 0.6-0.70 Mpa of high-purity nitrogen. Heating and stirring, the temperature in the kettle is raised to 80℃~85℃, and the pressure is increased from 0.6MPa to 3.3~3.5MPa. After reacting at this temperature and pressure for 10 hours, the material in the kettle is cooled to room temperature, and the unreacted The excess liquid ammonia is introduced into an absorption bottle filled with a sufficient amount of 25% sulfuric acid solution, and is emptied after absorption. Then, add 400ml of methanol to the kettle, stir, and discharge the material. The material is cooled to 0-5°C. A large amount of white crystals of ammonium chloride appear in the solution. Filter and collect the filtrate. Evaporate and remove methanol under normal pressure until the solution temperature ...

Embodiment 3

[0026] At room temperature, add 121g CMMO (1mol) to the 1.5L high-pressure ammoniation reactor, high-purity N 2 After sufficient replacement, 410 g of liquid ammonia (24 mol) was pressed into the reaction kettle using 0.6-0.70 MPa high-purity nitrogen. Heating and stirring, the temperature in the kettle is raised to 80℃~85℃, and the pressure is increased from 0.6MPa to 3.3~3.5MPa. After reacting at this temperature and pressure for 10 hours, the material in the kettle is cooled to room temperature, and the unreacted The excess liquid ammonia is introduced into an absorption bottle filled with a sufficient amount of 25% sulfuric acid solution, and after absorption, it is emptied. Then, add 400ml of diethyl ether and stir, discharge the material, cool the material to 0-5°C, a large amount of white crystals of ammonium chloride appear in the solution, filter, collect the filtrate, evaporate and remove the ether under normal pressure, until the temperature of the solution rises to...

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Abstract

The invention discloses a method for preparing 3-ammoniac methyl-3-methyl trimethylene oxide. The method takes 3-chloromethane radical-3-methyl trimethylene oxide (CMMO) and liquid ammonia as raw materials and comprises an ammoniation reaction and a post-treatment process. The method comprises the following steps: adding the CMMO into a high-pressure reaction kettle, using high-purity N2 to replace system air, using high-purity nitrogen to press the liquid ammonia into the reaction kettle, stirring and reacting for 8-12h at the temperature of 75-90 DEG C and the pressure of 3.2-4.0MPa; after finishing the ammoniation reaction, cooling the materials, taking out the excess liquid ammonia, adding an organic solvent into the reaction kettle, stirring, cooling the materials to 0-5 DEG C, filtering to remove existing crystals, collecting filtrate, evaporating to remove most of the solvent at normal pressure, cooling the materials to 0-5 DEG C again, filtering to remove the crystals in the materials, distilling the filtrate by depressurization and collecting distillates at 42-46 DEG C. A product obtained by the method is an organic intermediate for synthesizing medicines and pesticide.

Description

technical field [0001] The present invention relates to the preparation of 3-aminomethyl-3-methyloxetane. Background technique [0002] 3-Aminomethyl-3-methyloxetane (AmMMO) is an organic intermediate for the synthesis of medicines and pesticides, and is also the main raw material for the synthesis of difluoroaminooxetane energetic materials. JP 2007070270 reported a method for preparing AmMMO. Using pyridine and toluene as solvents, p-toluenesulfonyl chloride and 3-hydroxymethyl-3-methyloxetane were reacted at low temperature for 4 to 5 hours. A series of purification operations firstly prepare the intermediate of 3-methylene p-toluenesulfonate-3-methyloxetane, and then use it as a raw material to react with ammonia water at 100-110°C for 12 hours in a high-pressure reactor , and purified to obtain the target product. The preparation method has many reaction steps, lengthy and cumbersome process, needs to use toxic organic solvents such as pyridine, and has many three was...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D305/06
Inventor 张明权刘红雨高宝柱赵征康玲
Owner LIMING RES INST OF CHEM IND
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