Synthesis method of pheniramine maleate
A technology of pheniramine maleate and pheniramine maleate, which is applied in the field of synthesis of pheniramine maleate and can solve problems such as the lack of reports on the synthesis of pheniramine maleate
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Embodiment 1
[0018] Embodiment 1: the preparation of pheniramine maleate
[0019] (1) Preparation of benzylpyridine
[0020] Add 200g of phenylacetonitrile and 10g of catalyst cobaltocene into a 500ml autoclave, vacuumize, raise the temperature to 150°C, pass in dried acetylene gas, the temperature rises, keep the temperature at 150-170°C, pass in 100g of acetylene gas, and ventilate After the end, react under high pressure at 150-170°C for 4 hours. After the reaction, distill to obtain 260g of benzylpyridine.
[0021] (2) preparation of pheniramine maleate
[0022] Add 260g of benzylpyridine and 95g of sodium amide in tetrahydrofuran solvent, react at 20-25°C for 1 hour, then add dropwise the toluene solution of N,N-dimethyl chloride, and control the temperature at 30-40°C, After the dropwise addition, react at 40-45°C for 2 hours. After the reaction, cool down to normal temperature, then add water to wash the organic phase to neutrality, and recover the solvent to obtain the concentrat...
Embodiment 2
[0023] Embodiment 2: the preparation of pheniramine maleate
[0024] (1) Preparation of benzylpyridine
[0025] Add 200g of phenylacetonitrile and 8g of catalyst cobaltocene into a 500ml autoclave, vacuumize, raise the temperature to 140°C, pass in dried acetylene gas, the temperature rises, keep the temperature at 140-160°C, pass in 100g of acetylene gas, and ventilate After the end, react under high pressure at 150-160°C for 4.5h, after the end of the reaction, distill to obtain 270g of benzylpyridine.
[0026] (2) preparation of pheniramine maleate
[0027] In tetrahydrofuran solvent, add benzylpyridine 270g, sodium amide 100g, temperature is 20~25 ℃ and react for 1 hour, then dropwise add the toluene solution 282g (content 60%) of N,N-dimethyl chloride ethane, temperature control At 30-40°C, after the dropwise addition, react at 40-45°C for 2 hours, after the reaction, cool down to normal temperature, then add water to wash the organic phase until neutral, recover the so...
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