2-amino-2-phenylbutan-1-ol synthesis

Yield:39068-91-2 87.6%

Reaction Conditions:

with potassium borohydride;sulfuric acid in 1,2-dimethoxyethane at 15 - 20; for 10 h;Solvent;Reagent/catalyst;Temperature;

Steps:

1; 4-7 Example 6

The solvent ethylene glycol dimethyl ether 180g was put into a clean four-necked flask, and stirring was started, and 17.9g (0.1mol) of raw materials 2-amino-2-phenylbutyric acid and 13g (0.24mol) of potassium borohydride were added successively, Then, the temperature of the system was controlled at 15-20 °C under stirring, and 12.7 g (0.13 mol) of sulfuric acid was slowly added dropwise. After the dropwise addition, the reaction was kept at room temperature for 10 h. During the reaction, the intermediate control could be sampled. After the intermediate control was qualified, After the reaction finishes, the system temperature of the reaction solution is cooled to 10 , and then the mass percentage of 20% sodium hydroxide aqueous solution 60g (the addition of sodium hydroxide is 0.3mol) is added dropwise, and the dropwise temperature is controlled at 1015 . , the dropwise addition was completed, the temperature was raised to reflux for 2h, the heating was stopped and the layers were left to stand for stratification. The upper organic phase was collected, and the collected organic phase was concentrated under reduced pressure to recover the solvent to obtain the intermediate product 2-amino-2-phenylbutanol 14.4 g, pale yellow viscous liquid, GC content 98.3%, yield 87.6%.

References:

CN113999126,2022,A Location in patent:Paragraph 0030-0033; 0042-0043; 0046-0047; 0050-0051; ...