ChemicalBook CAS DataBase List 3,4-(Methylenedioxy)aniline

3,4-(Methylenedioxy)aniline synthesis

9synthesis methods

Product Name:3,4-(Methylenedioxy)aniline
CAS Number:14268-66-7
Molecular formula:C7H7NO2
Molecular Weight:137.14

3,4-Methylenedioxyaniline can be used as an intermediate for oxorilic acid in laboratory R&D processes. It can be synthesized by reduction of 1,2-(Methylenedioxy)-4-nitrobenzene.

2620-44-2
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$31.00/5g

14268-66-7
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$20.00/5G

Yield:14268-66-7 95.9%

Reaction Conditions:

with hydrogen;nickel in ethanol at 60; under 18751.9 Torr; for 2 h;Solvent;Pressure;Concentration;

Steps:

1 example one

The scalar quantity 81.9g (1.3mol) of 25% dilute nitric acid are added to a reaction tank, is heated to a certain temperature, the choice of temperature to a certain temperature as shown in table 1 ; in the reaction tank 0.4g/min speed slowly dropping 63.65g (0.52mol) 1,2-methylene-dioxy phongl, at the same time with 400r/min the speed of stirring vigorously, after dripping insulation 0.5 hours, cooling to 20 °C filtering to obtain the wet articles 3,4-methylenedioxy-nitrobenzene, purified water until pH value is neutral, the 40 °C vacuum 0.09 MPa drying under, to obtain 3,4-methylenedioxy-nitrobenzene intermediate, yield and purity is shown in table 1. The 3,4-methylenedioxy-nitrobenzene, skeleton nickel catalyst and ethanol are sequentially into the high-pressure reactor, air and then is discharged, the temperature rising to 60 °C hydrogen gas to begin when the, in 2.5 MPa pressure reaction introducing hydrogen into it; continuously under 2h, then intermittent introducing hydrogen into it; to until the hydrogen pressure does not change, reduced pressure distillation after filtering the catalyst, evaporate low boils the water and solvent and then high vacuum distillation, collecting 80-160Pa, 100-110 °C fraction, to get finished product 3,4-methylenedioxy-aniline, yield and purity is shown in table 1.

References:

CN105348251,2016,A Location in patent:Paragraph 0010; 0011

2635-13-4 Synthesis