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4964-49-2

1-(2-AMINOPHENYL)ETHAN-1-ONE OXIME synthesis

5synthesis methods
-

Yield:4964-49-2 90.3%

Reaction Conditions:

with hydroxylamine hydrochloride in ethanol at 80;Temperature;Concentration;

Steps:

4 Embodiment 4 of formula (VI) as shown in the synthesis of the compounds

For 500 ml is provided with a condensation return line, a thermometer in the four flasks are sequentially added ortho-amino-acetophenone 27g (0.2 μM), hydroxylamine hydrochloride 18.5g (0.266 μM), anhydrous ethanol 240 ml, 85 °C reflux, HPLC monitoring reaction; then cool to 20 °C, dropping 10% sodium carbonate solution, adjusting the pH=7.0 of the reaction solution, then the liquid is cooled to 10 °C, adding proper amount of water, the reaction solution becomes turbid, standing; then drop by almost 480 ml water, for 8 °C nourishing crystal 60 minutes; filtering, washing ethanol - water system, vacuum drying, get 27.09g white solid (VI) compound of formula, molar yield 90.3%, HPLC (%): 99.1%.

References:

CN104892609,2017,B Location in patent:Paragraph 0115; 0118; 0121; 0122; 0123; 0124

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