ChemicalBook CAS DataBase List Methoxymethyldiphenylamine

Methoxymethyldiphenylamine synthesis

10synthesis methods

Product Name:Methoxymethyldiphenylamine
CAS Number:41317-15-1
Molecular formula:C14H15NO
Molecular Weight:213.27

67-56-1 Synthesis

67-56-1
751 suppliers
$7.29/5ml-f

88-72-2
262 suppliers
$15.00/25g

108-95-2 Synthesis

108-95-2
739 suppliers
$14.00/25g

41317-15-1
210 suppliers
$41.00/25g

Yield:41317-15-1 95.4%

Reaction Conditions:

Stage #1:methanol;1-methyl-2-nitrobenzene with 3 % platinum on carbon;hydrogen in water at 50; under 750.075 Torr; for 8 h;Autoclave;Inert atmosphere;
Stage #2:phenol with 3 % platinum on carbon in cyclohexanone at 250; under 7500.75 Torr; for 2 h;Autoclave;Inert atmosphere;

Steps:

1.1-1.2 Example 1
(1) In a 200ml autoclave,Add 4.7ml of o-nitrotoluene,76.6ml of methanol, 2.7ml of distilled water,3% Pt / C0.02g,Seal the autoclave and replace the air 3 times with nitrogen.Pass in 0.1Mpa of hydrogen,Control the temperature at 50 for 8 hours.Stop the reaction, cool to room temperature, remove the reaction solution and filter.Most of the methanol was distilled off from the filtrate under reduced pressure. The residual solution was diluted with water and neutralized with ammonia to pH.Separate the upper organic phase, extract the aqueous phase three times with ether, combine the organic phases, and distill off the fractions under reduced pressure.MMA purity is 98.9%;
(2) In a 200ml autoclave,Add MMA26ml,106ml of phenol, 4.2ml of cyclohexanone,3% Pt / C0.28g,Seal the autoclave and replace the air in the autoclave with nitrogen.Then adjust the nitrogen pressure to 1Mpa,Control the temperature at 250 ° C for 2 hours.Cool to room temperature, take out the reaction solution and filter,The filtrate was distilled under reduced pressure, phenol was recovered, distillation was continued, DPA was distilled off, and recrystallization with ethanol to obtain 38.9 g of DPA,The yield was 95.4%.

References:

Hu Ting;Wang Cunliang;Xu Lingyan;Yan Xuewen;Huang Huanjun;Wang Xiaoqiao CN110642725, 2020, A Location in patent:Paragraph 0007

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27060-75-9 Synthesis