Process for preparing N-alkylarylamine
A technology of alkyl arylamine and alkyl group, applied in the field of preparation of N-alkyl arylamine, can solve the problems of instability, difficult separation of catalyst slurry and reaction product, hidden dangers of safe production and operation, etc.
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Embodiment 1
[0019] Embodiment 1: Preparation of 3-(N-benzyl)-amino-4-methoxy-acetanilide
[0020] 1. After drying 40-80 mesh silica gel at 110°C for 12 hours, add a certain amount of saturated nickel chloride solution to impregnate overnight, and then vacuum dry. Slowly add 2M potassium borohydride solution dropwise onto the silica gel carrier impregnated with nickel chloride until no bubbles are released. The obtained catalyst was washed with distilled water, soaked with ethanol, and put into a closed container for later use.
[0021] 2. In a 250ml stainless steel autoclave, add 100ml methanol, 18.5g 3-amino-4-methoxy-acetanilide (98.5%, 0.1mol), 12g benzaldehyde (99%, 0.11mol) and 1g step 1 in sequence Prepared supported Ni-B / SiO 2 Amorphous alloy catalyst. Seal the autoclave and pass in hydrogen to test for leaks, and replace it 4 to 5 times to remove the air in the autoclave. Flush in hydrogen gas again, start stirring at a stirring speed of 600 rpm, raise the temperature to 60° C...
Embodiment 2
[0022] Example 2: Preparation of 3-(N-p-tolylylene)-amino-4-methoxy-acetanilide
[0023] 1. Dried 40-80 mesh MCM-41 mesoporous molecular sieves at 110°C for 12 hours, then added a certain amount of saturated nickel chloride solution to impregnate overnight, and then dried in vacuum. Slowly add 2M potassium borohydride solution dropwise into the MCM-41 mesoporous molecular sieve carrier impregnated with nickel chloride until no bubbles are released. The obtained catalyst was washed with distilled water, soaked with ethanol, and put into a closed container for later use.
[0024] 2. In a 250ml stainless steel autoclave, add 100ml methanol, 18.5g 3-amino-4-methoxy-acetanilide (98.5%, 0.1mol), 16g p-tolualdehyde (98%, 0.11mol) and 2g step 1 Ni-B / MCM-41 amorphous alloy catalyst prepared. Seal the autoclave and pass in hydrogen to test for leaks, and replace it 4 to 5 times to remove the air in the autoclave. Flush in hydrogen gas again, start stirring at a stirring speed of 600 ...
Embodiment 3
[0025] Example 3: Preparation of 3-(N-benzyl)-amino-4-methoxy-acetanilide
[0026] 1. Dry 40-80 mesh silica gel at 110°C for 12 hours, add a certain amount of nickel chloride and palladium chloride solution to impregnate overnight, and then vacuum dry. Slowly add 2M potassium borohydride solution dropwise to the silica gel carrier impregnated with nickel chloride and palladium chloride until no bubbles are released. The obtained catalyst was washed with distilled water, then soaked with ethanol and placed in a closed container for future use.
[0027] 2. In a 250ml stainless steel autoclave, add 100ml ethanol, 18.5g 3-amino-4-methoxy-acetanilide (98.5%, 0.1mol), 12g benzaldehyde (99%, 0.11mol) and 0.5g step 1 Prepared Ni-Pd-B / SiO 2 catalyst. Seal the autoclave and pass in hydrogen to test for leaks, and replace it 4 to 5 times to remove the air in the autoclave. Flush in hydrogen again to reach the reaction pressure, start stirring at a stirring speed of 600 rpm, raise the...
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