ChemicalBook CAS DataBase List 3,4'-Oxydianiline

3,4'-Oxydianiline synthesis

7synthesis methods

Product Name:3,4'-Oxydianiline
CAS Number:2657-87-6
Molecular formula:C12H12N2O
Molecular Weight:200.24

22528-34-3

2657-87-6

GENERAL STEPS: The hydrogenation reaction was carried out in a 100 mL reaction flask equipped with an FB generator without additional stirring. 3-Amino-4'-nitrodiphenyl ether (10 mmol) was dissolved in ethyl acetate (80 mL) and subsequently heated to 30 °C. H2-FB was introduced into the reaction system in the presence of palladium alumina spheres (0.5% Pd, 2-4 mm, 0.3 mmol, 3 mol%) using a FB generator (MA3-FS) at a flow rate of 5 mL/min. The reaction progress was monitored by sampling the reaction periodically by GC analysis. Upon completion of the hydrogenation reaction, ethyl acetate was removed by vacuum evaporation to obtain high purity 3,4'-diaminodiphenyl ether.

22528-34-3 Synthesis

22528-34-3
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2657-87-6
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Yield:2657-87-6 > 99.9 %Spectr.

Reaction Conditions:

with 0.5% Pd on alumina;hydrogen in N,N-dimethyl-formamide at 30; for 7 h;Green chemistry;

Steps:

The typical procedure for hydrogenation of nitroarens using the H2-FB-based strategy:

General procedure: The hydrogenationwas carried out in a 100 mL vial equipped with an FB-generator without additional stirring. Nitroarene 1 (10mmol) was dissolved in ethyl acetate (80 mL), and then warmed to 30 °C. Using the FB-generator (MA3-FS), H2-FB was introduced into the reactor in the presence of palladium on alumina spheres (0.5%Pd, 2-4 mm, 0.3 mmol,3 mol%) at an H2-flow rate of 5 mL/min. The samples of the reaction mixture were taken out periodically tomonitor the reaction progress using the GC analysis. After the completion of the hydrogenation reaction, ethylacetate was evaporated in vacuo to afford the desired aniline 2 with good to excellent purity.

References:

Mase, Nobuyuki;Nishina, Yuki;Isomura, Shogo;Sato, Kohei;Narumi, Tetsuo;Watanabe, Naoharu [Synlett,2017,vol. 28,# 16,p. 2184 - 2188] Location in patent:supporting information