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ChemicalBook CAS DataBase List 4,4'-Methylenebis(2-methylcyclohexylamine)

4,4'-Methylenebis(2-methylcyclohexylamine) synthesis

2synthesis methods
Add 2000kg 3,3'-dimethyl-4,4'-diaminodiphenylmethane and 2000kg tetrahydrofuran to an autoclave with a volume of 6000L. Then, 100Kg 5% Ru/Al2O3 catalyst and 100Kg aluminum ammonium sulfate will be added, and the air in the autoclave will be replaced with hydrogen after sealing. Pour in 6MPa hydrogen, heat the autoclave to 160°C, adjust the hydrogen valve to maintain the pressure at 8MPa, and stir vigorously for 4 hours. After cooling, samples were taken and detected by gas chromatography-mass spectrometry. The detection results showed that the conversion rate of 3,3'-dimethyl-4,4-diaminodicyclohexylmethane was 100%, and the 4,4'-Methylenebis(2-methylcyclohexylamine) (MACM) yield was 99.4%.
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Yield:6864-37-5 99.4%

Reaction Conditions:

with ruthenium on aluminium oxide;ammonium aluminium sulfate;hydrogen in tetrahydrofuran at 160; under 60006 Torr; for 4 h;Acidic conditions;Large scale;

Steps:

10 Preparation of MACM from formula (IIb)

2000 kg of 3,3'-dimethyl-4,4'-diaminodiphenylmethane and 2000 kg of tetrahydrofuran were added to an autoclave having a volume of 6000 L, and then 100 kg of a 5% Ru/Al 2 O 3 catalyst and 100 kg of ammonium aluminum sulfate were added.After sealing, replace the air in the autoclave with hydrogen.Then, 6 MPa of hydrogen was introduced, and the autoclave was heated to 160 ° C. The hydrogen valve was adjusted to maintain the pressure in the autoclave at 8 MPa and the reaction was vigorously stirred for 4 hours.After cooling, sample and measure by gas chromatography-mass spectrometry.The detection result was that the conversion ratio of 3,3'-dimethyl-4,4'-diaminodiphenylmethane was 100%, and the MACM yield was 99.4%.

References:

CN108191671,2018,A Location in patent:Paragraph 0060-0062; 0072-0074

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