Method for synthesizing ticlopidine hydrochloride
A technology of ticlopidine hydrochloride and its synthetic method, which is applied in the field of organic compound synthesis, can solve problems such as unsuitability for industrialized production, influence on product yield, obsolete production process, etc., and achieve less environmental pollution, great promotion value, and production low cost effect
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Embodiment 1
[0037] Such as figure 2 The synthetic method of shown ticlopidine hydrochloride comprises the following steps:
[0038] 1. Protection of p-toluenesulfonyl group:
[0039] Add 500ml of toluene, 50g of thiophenethanol and 80g of p-toluenesulfonyl chloride into a 1000ml reaction bottle, start stirring, control the temperature and add 47g of triethylamine dropwise at 0°C, continue the dropwise addition for about 30min, and raise the temperature to 20°C for reaction 3 After 1 hour, add 400ml of water to the reaction solution, wash twice, and the toluene layer washed with water is directly used for the next step reaction.
[0040] 2. Condensation reaction
[0041] Add the toluene solution of the previous reaction into a 1000ml reaction bottle, then add 114g of o-chlorobenzylamine, heat up to 85°C and react for 3 hours, after the reaction, cool down to 20°C and stir for 1 hour, filter, add 200ml of water to the filtrate, stir Add hydrochloric acid dropwise to adjust the pH value ...
Embodiment 2
[0047] Such as figure 2 The synthetic method of shown ticlopidine hydrochloride comprises the following steps:
[0048] 1. Protection of p-toluenesulfonyl group:
[0049]Add 250ml of toluene, 25g of thiophene ethanol and 44g of p-toluenesulfonyl chloride into a 500ml reaction bottle, start stirring, and add 24g of triethylamine dropwise at 5°C under temperature control. The dropwise addition lasts for about 25min, and the temperature is raised to 25°C for reaction 1 After 1 hour, add 200ml of water to the reaction solution, wash in three times, and the toluene layer washed with water is directly used for the next step reaction.
[0050] 2. Condensation reaction
[0051] Add the toluene solution of the previous step into a 500ml reaction bottle, then add 70g of o-chlorobenzylamine, heat up to 80°C and react for 4 hours, after the reaction, cool down to 25°C and stir for 3 hours, filter, add 200ml of water to the filtrate, stir Add hydrochloric acid dropwise to adjust the pH...
Embodiment 3
[0057] Such as figure 2 The synthetic method of shown ticlopidine hydrochloride comprises the following steps:
[0058] 1. Protection of p-toluenesulfonyl group:
[0059] Add 500ml of toluene, 50g of thiophene ethanol and 84g of p-toluenesulfonyl chloride into a 1000ml reaction bottle, start stirring, and add 50g of triethylamine dropwise at 4°C under temperature control. The dropwise addition lasts for about 35min, and the temperature is raised to 22°C for reaction 2 After 1 hour, add 400ml of water to the reaction solution, wash twice, and the toluene layer washed with water is directly used for the next step reaction.
[0060] 2. Condensation reaction
[0061] Add the toluene solution of the previous step into a 1000ml reaction bottle, then add 126g of o-chlorobenzylamine, heat up to 95°C and react for 2 hours, after the reaction, cool down to 22°C and stir for 2 hours, filter, add 200ml of water to the filtrate, stir Add hydrochloric acid dropwise to adjust the pH valu...
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