Study On The Synthesis Technology Of 3-(1-Piperidinemethyl)Phenol

3-(1-Piperidinemethyl) Phenol is an important organic chemical intermediate. It’s widely used in pesticides, medicine, material and other fields, especially in the field of medicine,is an important intermediate for the synthesis of the anti-ulcer drug roxatidine series products. In this paper, m-hydroxybenzaldehyde was synthesized by one-pot syntheses process via successive reduction, diazo-reaction, hydrolysis reactions with m-nitrobenzaldehyde as the raw material. And I also researched the process conditions about m-hydroxybenzaldehyde and Piperidine as raw materials in the synthesis of 3-(1-Piperidinemethyl)Phenol.The optimum process conditions for one-pot syntheses process of m-hydroxybenzaldehyde from m-nitrobenzaldehyde:m-nitrobenzaldehyde 3.02 g (0.02 mol), the molar ratio of m-nitrobenzaldehyde and stannous chloride dehydrate is 1:3, reduction temperature 90 ℃, reduction time 90 min, hydrochloric acid 18mL, diazo-reaction temperature 10℃, diazo-reaction time 60 min, sodium nitrite 1.35g (0.0196mol), diazo-reaction feeding time 10 min, hydrolysis time 50 min. Under this condition, the yield can reach 63.97%, the purity can reach 98.53%."One-pot syntheses process" effectively shortens the reaction time, simplifies the operation steps, improves the production efficiency, further reduce the production cost.The optimum process conditions for preparing 3-(1-Piperidinemethyl)Phenol from m-hydroxybenzaldehyde and Piperidine:m-hydroxybenzaldehyde 2.442g (0.02 mol), the molar ratio of m-hydroxybenzaldehyde and Piperidine is 1:1.5, addition reaction time 1.5h, addition reaction temperature 40℃, sodium borohydride 0.908g (0.024 mol)(the molar ratio of m-hydroxybenzaldehyde and sodium borohydride is 1:1.2), reduction temperature 25℃, reduction time 9h. Under this condition, the yield can reach 73%, the purity can reach 100%.