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(2-Aminophenyl)-2-nitrophenyl ether synthesis

5synthesis methods
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Yield:91973-79-4 90%

Reaction Conditions:

with sodium hydride in N,N-dimethyl-formamide;mineral oil at 0 - 20; for 19 h;Inert atmosphere;

Steps:

3

5.00g in a 200ml three-necked flask under an argon atmosphere2-fluoronitrobenzene is dissolved in 50 ml of anhydrous dimethylformamide (THF).It was then cooled to about 0 °C. Then, 3.86 g of 2-aminophenol and 2.83 g of sodium hydride (60% in oil) were added thereto. Stir about 1 hour at about 0 ° CAfter the time, carry out stirring for about 18 hours while slowly bringing the temperatureReturn to room temperature. After the reaction is completed, water is added at about 0 ° C.It was extracted with dichloromethane (CH 2 Cl 2 ). With magnesium sulfate (MgSO4)After drying, the solvent was distilled and removed under pressure. The crude product thus obtained was separated by silica gel column chromatography to give 7.34 g (yield: 90%)Intermediate K.

References:

CN109553634,2019,A Location in patent:Paragraph 0219-0222; 0224