A kind of method for preparing 2-amino-2-methyl-1-propanol
A technology of methylpropionitrile and methyl, which is applied in the field of preparing 2-amino-2-methyl-1-propanol, can solve the problems of complex process, limited source of raw materials, complicated preparation steps, etc., and achieve simple reaction process, Obvious cost advantage and product purification effect
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Embodiment 1
[0035] Weigh 117g of sodium cyanide and grind it finely, add it to 120g of water at room temperature, and stir until the sodium cyanide is completely dissolved. Weigh 157g of 2-chloropropane and 160g of ethanol and mix them, then slowly drop them into the aqueous sodium cyanide solution, and after the dropwise addition, raise the temperature to 95°C for 4 hours. Cool down after the end of the reaction, filter and remove the precipitated sodium chloride solid, wash the filtrate twice with about 20g ethanol, combine the filtrate and carry out distillation to remove ethanol and water, filter again to remove sodium cyanide and sodium chloride precipitation, obtain 141g thick 2-formazan propionitrile, the purity is about 87.9%, and the target product yield of this step is about 90%.
[0036] Crude 2-methylpropionitrile was mixed with 182g 37wt% formaldehyde aqueous solution, and 21g 30wt% trimethylamine aqueous solution was added dropwise under stirring, and reacted at 45°C for 1.5...
Embodiment 2
[0041] Weigh 98g of sodium cyanide and grind it finely, add it into 53g of water at room temperature, and stir until the sodium cyanide is completely dissolved. Weigh 157g of 2-chloropropane and 85g of ethanol and mix them, then slowly drop them into the aqueous sodium cyanide solution, and after the dropwise addition, raise the temperature to 80°C for 8 hours of reaction. Cool down after the end of the reaction, filter and remove the precipitated sodium chloride solid, wash the filtrate twice with about 20g of ethanol, combine the filtrate and carry out distillation to remove ethanol and water, filter again to remove sodium cyanide and sodium chloride precipitation, obtain 142g thick 2-formazan propionitrile, the purity is about 82.4%, and the target product yield of this step is about 84.8%.
[0042] Crude 2-methylpropionitrile was mixed with 172g of 37% formaldehyde aqueous solution, 30g of 30wt% trimethylamine aqueous solution was added dropwise under stirring, and reacted...
Embodiment 3
[0047] Weigh 127g of sodium cyanide and grind it finely, add it into 237g of water at room temperature, and stir until the sodium cyanide is completely dissolved. Weigh 157g of 2-chloropropane and 290g of ethanol and mix them, then slowly drop them into the aqueous sodium cyanide solution, and after the dropwise addition, raise the temperature to 105°C for 3 hours of reaction. Cool down after reaction finishes, filter and remove the sodium chloride solid that separates out, wash filtrate twice with about 20g ethanol, combine filtrate and carry out distillation and remove ethanol and water, filter again and remove sodium cyanide and sodium chloride precipitation, obtain 139.4g thick 2- Methylpropionitrile has a purity of about 87.1%, and the yield of the target product in this step is about 88%.
[0048] Crude 2-methylpropionitrile was mixed with 150g of 37wt% formaldehyde aqueous solution, 5.3g of triethylamine was added dropwise under stirring, and reacted at 60°C for 50min. ...
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