Novel preparation method for ticlopidine hydrochloride
A technology of ticlopidine hydrochloride and a new method, which is applied in the field of organic compound synthesis, can solve problems such as not being suitable for industrial production, affecting product yield, and obsolete production technology, and achieve less environmental pollution, great promotion value, and production low cost effect
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Embodiment 1
[0036] like figure 2 Shown is the new method for preparing ticlopidine hydrochloride, comprising the following steps:
[0037] 1. Protection of p-toluenesulfonyl group:
[0038] Add 500ml of toluene, 50g of thiophene ethanol and 92g of p-toluenesulfonyl chloride into a 1000ml reaction bottle, start stirring, and add 62g of N,N-diisopropylethylamine dropwise at 0°C under temperature control, and the dropwise addition lasts about 30min. After dropping, the temperature was raised to 20°C for 3 hours, and 400ml of water was added to the reaction solution, which was washed twice, and the toluene layer washed with water was directly used for the next reaction.
[0039] 2. Condensation reaction
[0040] 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 hydrochlori...
Embodiment 2
[0046] like figure 2 Shown is the new method for preparing ticlopidine hydrochloride, comprising the following steps:
[0047] 1. Protection of p-toluenesulfonyl group:
[0048]Add 250ml of toluene, 25g of thiophene ethanol and 42g of p-toluenesulfonyl chloride into a 500ml reaction bottle, start stirring, and add 30g of N,N-diisopropylethylamine dropwise at 5°C under temperature control, and the dropwise addition lasts for about 25min. After dripping, raise the temperature to 25°C for 1 hour reaction, add 200ml of water to the reaction solution, and wash it three times. The toluene layer washed with water is directly used for the next step reaction.
[0049] 2. Condensation reaction
[0050] 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 dr...
Embodiment 3
[0056] like figure 2 Shown is the new method for preparing ticlopidine hydrochloride, comprising the following steps:
[0057] 1. Protection of p-toluenesulfonyl group:
[0058] Add 500ml of toluene, 50g of thiophene ethanol and 88g of p-toluenesulfonyl chloride into a 1000ml reaction flask, start stirring, and add 59g of N,N-diisopropylethylamine dropwise at 4°C under temperature control, and the dropwise addition lasts for about 35min. After dropping, the temperature was raised to 22°C for 2 hours, and 400ml of water was added to the reaction solution, which was washed twice, and the toluene layer washed with water was directly used for the next reaction.
[0059] 2. Condensation reaction
[0060] 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 hydrochlori...
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