Preparation method of methyl 4-acetylaminomethyl hexahydrobenzoate
A technology of methyl acetamidomethyl cyclohexyl formate and methyl acetamidomethyl benzoate, applied in the field of preparation of methyl 4-acetamidomethyl cyclohexyl formate, can solve the problems of expensive catalyst and high cost, and achieves The effect of simplifying the post-processing process, low cost, and reducing the difficulty of separation
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Embodiment 1
[0030] (1) Preparation of methyl paraacetamidomethyl benzoate
[0031] Add methyl p-cyanobenzoate (40.0g, 0.248mol, purity 97.6606%), acetic anhydride, 260mL, catalyst Pd / C 2.0g, promoter anhydrous potassium acetate 12g, and close the reactor to a 1L hydrogenation kettle. Replace the air with 1MPa hydrogen for 3 times (or replace with nitrogen), and then pass 1MPa hydrogen for leak detection. If there is no leakage, adjust the pressure to 0.3MPa and start stirring at 20°C to react. When the hydrogen drops by 0.2MPa, make up Hydrogen to 0.3MPa, react for 6 hours until the hydrogen pressure no longer drops, stop the reaction, open the kettle, filter the reaction liquid, and distill the filtrate to recover acetic acid and acetic anhydride to obtain white solid methyl paraacetamido methyl benzoate with a mass of 42.43 g, mp: 113-114°C, molar yield 82.65%. 1H NMR (400 MHz, CDCl3) δ 2.05 (s, 3H), 3.90 (s, 3H), 4.47 (d, J = 5.9Hz, 2H), 6.02 (s, 1H), 7.31 (d, J = 8.1Hz , 2H), 7.96 (d, ...
Embodiment 2
[0037] (1) Preparation of methyl paraacetamidomethyl benzoate
[0038] Add methyl p-cyanobenzoate (30.0g, 0.186mol, purity 97.6606%), 220mL of acetic anhydride, catalyst aluminum-nickel alloy powder (with nickel content greater than or equal to 45%), 6.0g, and co-catalyst into a 1L hydrogenation kettle 22g of anhydrous sodium acetate, close the reactor, pass 1MPa hydrogen to replace the air 3 times (or replace with nitrogen), and then pass 1MPa hydrogen to check for leaks. If there is no leakage, adjust the pressure to 0.8MPa, turn on stirring and heat up to 54 °C reaction. When the hydrogen drops by 0.2 MPa, make up hydrogen to 0.8 MPa, react for 6 hours until the hydrogen pressure no longer drops, stop the reaction, open the kettle, filter the reaction liquid, and distill the filtrate to recover acetic acid and acetic anhydride to obtain a white solid p-acetaminomethyl Methyl benzoate, mass 28.27g, mp: 113-114°C, molar yield 73.42%.
[0039] (2) Preparation of methyl 4-acetylam...
Embodiment 3
[0042] (1) Preparation of methyl paraacetamidomethyl benzoate
[0043] Add methyl p-cyanobenzoate (36.0g, 0.224mol, purity 97.6606%), acetic anhydride 240mL, catalyst Raney nickel 12.6g, promoter anhydrous potassium acetate 43.2g into the 1L hydrogenation kettle, close the reactor , Replace the air with 1MPa hydrogen for 3 times (or replace with nitrogen), and then pass 1MPa hydrogen to check for leaks. If there is no leakage, adjust the pressure to 1.5MPa, turn on the stirring and increase the temperature to 70°C for reaction. When the hydrogen drops by 0.2MPa, make up the hydrogen to 1.5MPa, react for 10 hours until the hydrogen pressure does not drop, stop the reaction, open the kettle, filter the reaction liquid, and distill the filtrate to recover acetic acid and acetic anhydride to obtain a white solid paraacetaminomethyl Methyl benzoate, mass 32.61g, mp: 113-114°C, molar yield 70.32%.
[0044] (2) Preparation of methyl 4-acetylaminomethylcyclohexylcarboxylate
[0045] Add me...
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