Preparation method of 2-amino-2-methyl-1-propanol
A technology of amino and methyl, which is applied in the field of preparation of 2-amino-2-methyl-1-propanol, which can solve the problems of large production investment, high risk of synthetic raw materials, and difficult purification of products, and achieve small equipment volume , cheap raw materials, low cost effect
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Embodiment 1
[0025] 205.5g of acetonitrile (5mol) is loaded into a 500ml glass tube reactor, the two ports of the reaction bottle are connected to the bottom tube, one is connected to the chlorine gas source, the other is connected to the isobutylene source, and the other is equipped with a thermometer. Put it into an ice-water bath at 0°C, start magnetic stirring, wait until the temperature of the system drops to 0°C, and at the same time, pass 63.8g (0.9mol) of chlorine gas and 50.5g (0.9mol) of isobutene into the reaction flask according to the same ratio. Continue to stir for half an hour after ventilating, then add 11 g of water (0.6 mol) dropwise, stir for half an hour after the dropwise addition, then filter, and vacuum concentrate the filtrate at about 45° C. to obtain 83 g of a slightly yellow concentrate. Dissolve the concentrated solution obtained in the previous step with 41.5 g of ethanol solution with a volume concentration of 95%, heat and stir until it refluxes, then add 29....
Embodiment 2
[0028]205.5g of acetonitrile (5mol) is loaded into a 500ml glass tube reactor, the two ports of the reaction bottle are connected to the bottom tube, one is connected to the chlorine gas source, the other is connected to the isobutylene source, and the other is equipped with a thermometer. into a 30°C water bath, and at the same time 39g (0.55mol) of chlorine and 30.86g (0.55mol) of isobutene were slowly passed into the reaction flask. Continue to stir for half an hour after ventilating, then add 11g of water (0.6mol) dropwise, (hydrolysis reaction exotherm) and stir for half an hour after dropwise addition, then filter, and vacuum concentrate the filtrate at about 45°C to obtain 57g of a yellowish concentrate. Dissolve the concentrated solution obtained in the previous step with 28.5 g of ethanol with a volume concentration of 95%, heat and stir until it refluxes, then add 19.95 g of concentrated hydrochloric acid with a mass concentration of 37%, heat and reflux for about 2 h...
Embodiment 3
[0031] In the glass reactor of 500ml, the acetonitrile (7.23mol) of packing 297g, two ports of reaction flask are connected with inserting bottom pipe, one connects chlorine gas source, one connects isobutylene source, another mouth is equipped with thermometer, puts reaction flask into- In an ice-salt bath at 10°C, 34.8g (0.62mol) of chlorine gas and 46g (0.65mol) of isobutene were slowly passed into the reaction flask at the same time. Continue to stir for half an hour after ventilating, add 15g of water (0.833mol) dropwise, (hydrolysis reaction exotherm) and stir for half an hour after dropwise addition, then filter, and vacuum concentrate the filtrate at about 45°C to obtain 93g of slightly yellow concentrate. Dissolve the concentrated solution obtained in the previous step with 46.5 g of ethanol with a volume concentration of 95%, then heat and stir until reflux, then add 32.55 g of concentrated hydrochloric acid with a mass concentration of 37%, heat to reflux for about 2...
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