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ChemicalBook CAS DataBase List 4-Nitrobenzeneethanol

4-Nitrobenzeneethanol synthesis

13synthesis methods
-

Yield:100-27-6 96.5%

Reaction Conditions:

with lithium aluminium tetrahydride in diethyl ether at 50; for 3 h;Inert atmosphere;Temperature;

Steps:

2 Example 2

(1) Dissolve p-nitrophenylacetic acid in ether.Heat to 50°C under nitrogen protectionAfter adding lithium aluminum hydride and mixing evenly,Add water, continue stirring for 3h,After the reaction is completed,Reduce the temperature to 0 °C,Add sodium hydroxide solution and water,The concentration of sodium hydroxide solution is 12%.After standing for 20 minutes, warm to room temperature and add anhydrous MgSO4.After stirring for 30min,The solvent in the filtrate is distilled off,Obtained p-nitrophenyl ethanol;(2) dissolving the obtained p-nitrophenyl ethanol in ethanol,The catalyst was added, nitrogen was introduced, and the temperature was raised to 80°C.Hydrogen gas is introduced under atmospheric pressureStir the reaction for 3h,Filter after cooling,Ethanol is distilled,After the resulting solid is recrystallized,Obtained p-aminophenyl ethanol;The catalyst is a mixture of CeO2, MnO, and ZnO.The mass ratio of lithium aluminum hydride used in step (1) to p-nitrophenylacetic acid is 1:2; the volume of water added dropwiseThe mass ratio to lithium aluminum hydride is 1:1; the mass ratio of sodium hydroxide to lithium aluminum hydride is 3:2 and the second additionThe mass ratio of water to lithium aluminum hydride is 5:2.The catalyst in step (2) is a mixture of CeO2, MnO and ZnO in a mass ratio of 1:2:5;The mass ratio of nitrobenzene ethanol is 3:167. The step (1)

References:

CN108033888,2018,A Location in patent:Paragraph 0019-0057

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