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ChemicalBook CAS DataBase List 2-Amino-2-methyl-1-propanol
124-68-5

2-Amino-2-methyl-1-propanol synthesis

11synthesis methods
The synthesis of 2-Amino-2-methyl-1-propanol is as follows:

In a 1L three-neck flask with mechanical stirring, first add 200ml of water, add a few drops of dilute sulfuric acid to make it slightly acidic (pH=3.5-4), then heat to 40-50, and start adding 99.0 at the same time. 2,2-Dimethylaziridine and 400ml dilute sulfuric acid aqueous solution, keep the temperature and slightly acidic condition, drop 2,2-dimethylaziridine, then continue to react at this temperature 1h, then under reduced pressure distillation to remove 80% of the water, add 500ml ethanol to the obtained system, neutralize with 30% sodium hydroxide to pH=9.5-10, filter and remove the salt, the obtained filtrate is distilled out of ethanol under normal pressure , And then distilled under reduced pressure to obtain crude 2-amino-2-methyl-1-propanol. This crude product is then rectified to obtain 112.9g 2-amino-2-methyl-1-propanol refined product with a yield of about 91.0%, chromatographic purity is about 99.4%.
124-68-5.png

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Yield:124-68-5 103 g

Reaction Conditions:

with sodium hypochlorite;sodium hydroxide in water at 0 - 70; for 0.333333 h;Hofmann Rearrangement;Temperature;

Steps:

1 Example 1

109 g of sodium hypochlorite and 106 g of sodium hydroxide were weighed and dissolved in 600 g of water. The above solution was dissolved in a temperature of about 0 ° C,The crude product of 2,2-dimethyl-3-hydroxypropionamide was added dropwise with stirring, and the temperature was raised to 70 ° C for 20 min. After the reaction is overThe water was distilled off, and the mixture was purified by filtration to obtain 103 g of 2-amino-2-methyl-1-propanol and 99.2 wt% purity.The target product yield was about 86.3%.The total yield of 2-amino-2-methyl-1-propanol was about 57.4%.

References:

CN107129435,2017,A Location in patent:Paragraph 0034; 0038; 0039; 0044; 0045; 0050; 0051

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