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Technology for producing aminoacetaldehyde dimethyl acetal

A technology of aminoacetaldehyde dimethyl acetal and chloroacetaldehyde dimethyl acetal is applied in the preparation of amino hydroxy compounds, the preparation of organic compounds, organic chemistry, etc., and can solve energy consumption, separation of air difficulties, and separation of aminoacetaldehyde dimethyl acetal. Difficulties and other problems to achieve the effect of reducing demand and reducing consumption

Inactive Publication Date: 2019-07-16
INNER MONGOLIA SAINTCHEM CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the produced aminoacetaldehyde dimethyl acetal conjugate is useless and difficult to separate from aminoacetaldehyde dimethyl acetal, this process brings corresponding environmental problems and energy consumption
At the same time, the separation of aminoacetaldehyde dimethyl acetal and water caused a large amount of energy consumption by high-tower rectification

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1 In a 3000L autoclave, an aqueous ammonia solution containing carbon dioxide was put in, with a total weight of 1445 kg, which contained 410 kg, 24.12 kmol of ammonia, 900 kg, 50 kmol of water, and 135 kg, 3.07 kmol of carbon dioxide. Then use a metering pump to add chloroacetaldehyde dimethyl acetal to the kettle, the quality of chloroacetaldehyde dimethyl acetal is 100kg, 0.8 kmol. Reaction at 140°C for 7 hours, after pressure relief and cooling, after deamination at 90°C under normal pressure, cool down to 30°C, drop 30% liquid caustic soda from the metering tank: 107kg to the dehydration kettle, after the dropwise addition, stir for 0.5 h, continue to heat up to 150°C, distill the crude product, and obtain 76.9kg of the finished product through rectification, with a reaction molar yield of 90.47%.

Embodiment 2

[0015] Embodiment 2, in a 3000L autoclave, drop into the aqueous ammonia solution that contains carbon dioxide, gross weight is 1455 kilograms, wherein contains ammonia 410kg, 24.12kmol, water 900 kg, 50 kmol, carbon dioxide 145kg, 3.30kmol. Then use a metering pump to add chloroacetaldehyde dimethyl acetal to the kettle, the quality of chloroacetaldehyde dimethyl acetal is 100kg, 0.8 kmol. Reaction at 140°C for 5 hours, after pressure relief and cooling, after deamination at 90°C under normal pressure, cool down to 30°C, drop 30% liquid caustic soda from the metering tank: 107kg to the dehydration kettle, after the dropwise addition, stir for 0.5 h, continue to heat up to 150°C, distill the crude product, and obtain 77.62kg of the finished product through rectification, with a reaction molar yield of 91.32%.

Embodiment 3

[0016] Embodiment 3, in a 3000L autoclave, drop into the aqueous ammonia solution that contains carbon dioxide, gross weight is 1705 kilograms, wherein contains ammonia 460kg, 27.06kmol, water 1100 kg, 61.11 kmol, carbon dioxide 145kg, 3.30kmol. Then use a metering pump to add chloroacetaldehyde dimethyl acetal to the kettle, the quality of chloroacetaldehyde dimethyl acetal is 100kg, 0.8kmol. Reaction at 140°C for 8 hours, after pressure relief and cooling, after deamination at normal pressure at 90°C, cool down to 30°C, drop 30% liquid caustic soda from the metering tank: 107kg to the dehydration kettle, after the dropwise addition, stir for 0.5 h, continue to heat up to 150°C, distill the crude product, and obtain 80.07kg of the finished product through rectification, with a reaction molar yield of 94.20%.

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Abstract

The invention discloses a new technology for producing aminoacetaldehyde dimethyl acetal. Chloroacetaldehyde dimethyl acetal is firstly synthesized into aminoacetaldehyde dimethyl acetal by using ammonia solution containing carbon dioxide, aminoacetaldehyde dimethyl acetal and carbon dioxide are then converted to hydroxymethyl aminopropyl formic acid, aminoacetaldehyde dimethyl acetal is preventedfrom continuously reacting with chloroacetaldehyde dimethyl acetal to generate secondary and tertiary amine, after deamination, hydroxymethyl propylcarbamic acid is decomposed into aminoacetaldehydedimethyl acetal and carbon dioxide after high temperature and acid aqueous reflux. After recovering carbon dioxide, aminoacetaldehyde dimethyl acetal hydrochloride is obtained, and then aminoacetaldehyde dimethyl acetal hydrochloride is neutralized, distilled and rectified to obtain high purity aminoacetaldehyde dimethyl acetal.

Description

technical field [0001] The invention relates to a production process of aminoacetaldehyde dimethyl acetal, which is obtained by using chloroacetaldehyde dimethyl acetal and ammonia water as raw materials and using carbon dioxide as a catalyst through ammoniation, deamination, dehydration, neutralization, distillation and rectification. Synthetic process of high-purity aminoacetaldehyde dimethyl acetal. Background technique [0002] Aminoacetaldehyde dimethyl acetal, also known as aminoacetaldehyde dimethyl acetal, has a molecular formula of C4H12NO2, a molecular weight of 106.143, and a CAS registration number of 22483-09-6. It is a colorless liquid used as a pharmaceutical intermediate . It is used in the effective synthesis of proline analogues from ascorbic acid through a 3-step reaction; it is also used to prepare phosphoramidates with a 3-step reaction catalyzed by MgClO4. [0003] The traditional process of aminoacetaldehyde dimethyl acetal takes the route of directl...

Claims

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Application Information

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IPC IPC(8): C07C217/40C07C213/02
CPCC07C213/02C07C217/40
Inventor 白深科杨丰乐马骅
Owner INNER MONGOLIA SAINTCHEM CHEM
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