Synthetic method of 2-((1-benzyl-4-piperidyl)-hydroxy-methyl)-5, 6-dimethoxy-1-indanone
A technology of dimethoxy, benzyl piperidine, applied in the field of organic synthesis, can solve the problems of insufficient reduction of pyridine ring, increased production cost of enterprises, low purity of target product, etc., achieves easy control, reduced production cost, and improved production The effect of high safety
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[0016] A kind of synthetic method of 2-((1-benzyl-4-piperidinyl)-hydroxyl-methyl)-5,6-dimethoxy-1-indanone according to the present invention comprises the following steps :
[0017] ①Use methanol, thionyl chloride, and 4-piperidinecarboxylic acid to synthesize methyl 4-piperidinecarboxylic acid, use benzyl chloride as benzyl and triethylamine for benzylation to obtain N-benzyl-4-piperidinecarboxylic acid Methyl ester, the mass ratio of materials used is: methyl alcohol: thionyl chloride: 4-piperidinecarboxylic acid: benzyl chloride: the ratio of triethylamine is 6.67:3.08:1:1:1.52;
[0018] ② Use N-benzyl-4-piperidinecarboxylic acid methyl ester and 5,6-dimethoxy-1-indanone to obtain 2-(1-benzylpiperidine-4-carbonyl)-5 , 6-dimethoxy-1-indanone, the mass ratio of the materials used is: methyl N-benzyl-4-piperidinecarboxylate: the ratio of sodium methoxide (25% methanol solution) is 1.4:1.13;
[0019] ③Reduce 2-(1-benzylpiperidine-4-carbonyl)-5,6-dimethoxy-1-indanone with sod...
Embodiment 1
[0023] Specific steps are as follows:
[0024] ①Preparation of methyl N-benzyl-4-piperidinecarboxylate: put 100kg of methanol into the reaction kettle, add 46.24kg of thionyl chloride dropwise under temperature control at 15°C, add 15kg of 4-piperidinecarboxylic acid after the dropwise addition, Keep warm at 15°C for 30 minutes, then raise the temperature to 25°C for 20 hours, evaporate the solvent under reduced pressure after the reaction, wash the solid with 15kg of isopropyl ether, filter and dry in vacuum for 4 hours, add 100kg of di Chloromethane, after cooling to 10°C with ice water, add 14.96kg of benzyl chloride dropwise, the reaction temperature is controlled at 10°C, after the benzyl chloride has been added dropwise, add 22.86kg of triethylamine dropwise, and keep warm at 10°C for 30 minutes. Raise the temperature to 25°C and react for 20 hours. After the reaction, the solvent was evaporated under reduced pressure, and the oil was washed twice with 30 kg of water, an...
Embodiment 2
[0028] Specific steps are as follows:
[0029]①Preparation of methyl N-benzyl-4-piperidinecarboxylate: put 100kg of methanol into the reaction kettle, add 46.24kg of thionyl chloride dropwise under temperature control at 15°C, add 15kg of 4-piperidinecarboxylic acid after the dropwise addition, Keep warm at 15°C for 30 minutes, then raise the temperature to 25°C for 20 hours, evaporate the solvent under reduced pressure after the reaction, wash the solid with 15kg of isopropyl ether, filter and dry in vacuum for 4 hours, add 100kg of di Chloromethane, after cooling to 10°C with ice water, add 14.96kg of benzyl chloride dropwise, the reaction temperature is controlled at 10°C, after the benzyl chloride has been added dropwise, add 22.86kg of triethylamine dropwise, and keep warm at 10°C for 30 minutes. Raise the temperature to 25°C and react for 20 hours. After the reaction, the solvent was evaporated under reduced pressure, and the oil was washed twice with 30 kg of water, and...
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