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ChemicalBook CAS DataBase List Aminoacetaldehyde dimethyl acetal
22483-09-6

Aminoacetaldehyde dimethyl acetal synthesis

5synthesis methods
1) to disposable in container, add the ammonia soln that monochloroacetaldehyde dimethyl acetal and concentration are 10~40%, stir;
2) by step 1) in reaction solution stir, this reaction solution is warming up to 100~150 ℃;
3) by step 2) in reaction solution distill, reclaim ammoniacal liquor, until steam without obvious cut;
4) in step 3) in reaction solution in to add concentration be 20%~50% aqueous sodium hydroxide solution, regulate pH to 12~14;
5) by step 4) in solution carry out rectifying, collect colourless and light yellow transparent liquid, be target product aminoacetaldehyde dimethyl acetal.
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Yield:22483-09-6 94.2%

Reaction Conditions:

with ammonium hydroxide;carbon dioxide at 140; for 8 h;Autoclave;Large scale;

Steps:

1-3 In Example 3

in a 3000 L autoclave, an aqueous ammonia solution containing carbon dioxide was introduced, and the total weight was 1,705 kg, which contained 460 kg of ammonia, 27.06 kmol, water of 1100 kg, 61.11 kmol, carbon dioxide of 145 kg, and 3.30 kmol. Then, chloroacetaldehyde dimethyl acetal was introduced into the kettle using a metering pump, and the mass of chloroacetaldehyde dimethyl acetal was 100 kg, 0.8 kmol. After reacting at 140 ° C for 8 hours, after depressurization and cooling, after deamination at normal pressure of 90 ° C, the temperature is lowered to 30 ° C, and 30% of liquid alkali: 107 kg is added from the measuring tank to the dehydration kettle. After the addition is completed, the mixture is stirred. h, continue to raise the temperature to 150 ° C, distill off the crude product, the crude product is rectified to obtain the finished product 80.07 kg, the reaction molar yield is 94.20%.

References:

CN110015964,2019,A Location in patent:Paragraph 0014-0016

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