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Preparation method of benserazide hydrochloride impurity

A technology of benserazide hydrochloride and impurities, which is applied in the field of medicine and can solve problems such as low efficiency, waste, and poor stability

Active Publication Date: 2020-08-04
SHANGHAI SYNCORES TECH INC +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method is inefficient, time-consuming, and wasteful
The more important reason is that the impurity itself is not stable, and most of it will be destroyed in the process of separation and concentration
[0009] To sum up, this impurity, as a pharmacopoeia impurity, needs to be used as a standard product for positioning and content inspection in daily testing, but currently there is no efficient and convenient synthesis or separation method that can prepare a large-scale technical means for this impurity standard product

Method used

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  • Preparation method of benserazide hydrochloride impurity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 9.6g of benserazide hydrochloride and 30ml of water into a 100ml three-necked flask, heat to 20-30°C and stir for 16-20 hours, then concentrate to remove water. Add 20mL of methanol, lower the temperature to 0-10°C, add 80mL of ethanol dropwise, precipitate a solid and keep stirring, then suction filter to obtain the crude product. Add 20mL of methanol and 10mL of water to the crude product at 10-20°C and stir to dissolve, then add dropwise 30mL of ethanol to stir and crystallize, filter and dry to obtain Pharmacopoeia Impurity B of Benserazide Hydrochloride, 4.1g, yield 55.5%. 1 H NMR (400 MHz, DMSO-d 6 )δ9.83(s,1H),8.76(s,2H),8.16(s,4H),6.35(d,J=8.3Hz,2H),6.14(d,J=8.2Hz,2H),5.39( t,J=4.9Hz,1H),4.30(d,J=4.1Hz,1H),3.81–3.64(m,1H),3.73(d,4H),3.51–3.33(m,2H).Mass:396.1 [M+H].

Embodiment 2

[0022] Add 2.0g of benserazide hydrochloride and 6ml of water into a 100ml three-necked flask, heat to 30-40°C and stir for 6-8 hours, then concentrate to remove water. Add 30mL of methanol, lower the temperature to 0-10°C, precipitate a solid, heat it and stir it, then filter it with suction to obtain the crude product. Add 20mL of methanol and 10mL of water to the crude product at 10-20°C and stir to dissolve, then dropwise add 30mL of methanol to stir and crystallize, filter and dry to obtain Pharmacopoeia impurity B of benserazide hydrochloride, 0.82g, yield 53.2%. 1 H NMR (400MHz, DMSO-d 6 )δ9.83 (s, 1H), 8.76 (s, 2H), 8.16 (s, 4H), 6.35 (d, J = 8.3Hz, 2H), 6.14 (d, J = 8.2Hz, 2H), 5.39 ( t,J=4.9Hz,1H),4.30(d,J=4.1Hz,1H),3.81–3.64(m,1H),3.73(d,4H),3.51–3.33(m,2H).Mass:396.1 [M+H].

Embodiment 3

[0024] Add 2.0g of benserazide hydrochloride and 6ml of water into a 100ml three-necked flask, heat to 30-40°C and stir for 6-8 hours, then concentrate to remove water. Add 30mL of ethanol, lower the temperature to 0-10°C, precipitate a solid, heat it and stir it, then filter it with suction to obtain the crude product. Add 20mL of ethanol and 10mL of water to the crude product at 10-20°C and stir to dissolve, then add dropwise 30mL of ethanol to stir and crystallize, filter and dry to obtain Pharmacopoeia impurity B of benserazide hydrochloride, 0.88g, yield 57.1%. 1 H NMR (400MHz, DMSO-d 6 )δ9.83 (s, 1H), 8.76 (s, 2H), 8.16 (s, 4H), 6.35 (d, J = 8.3Hz, 2H), 6.14 (d, J = 8.2Hz, 2H), 5.39 ( t,J=4.9Hz,1H),4.30(d,J=4.1Hz,1H),3.81–3.64(m,1H),3.73(d,4H),3.51–3.33(m,2H).Mass:396.1 [M+H].

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Abstract

The invention discloses a preparation method of a benserazide hydrochloride impurity, and particularly relates to a preparation method of a benserazide hydrochloride pharmacopeia impurity B. The method is simple and easy to operate, mild in condition, high in yield, low in energy consumption and pollution and suitable for preparing laboratory-level standard substances.

Description

technical field [0001] The invention reports a preparation method of benserazide hydrochloride impurity, specifically a preparation method of benserazide hydrochloride pharmacopoeia impurity B, which belongs to the field of medicine. Background technique [0002] Benserazide Hydrochloride is an active ingredient in the compound drug Madopar for the treatment of Parkinson's. The original research company of Madopar is Roche Pharmaceuticals, and the active ingredients are levodopa and benserazide hydrochloride. This drug can increase the content of dopamine in brain cells and improve Parkinson's symptoms. Benserazide hydrochloride is a dopa decarboxylase (Dopa decarboxylase) inhibitor, which can block the conversion of levodopa into dopamine before it enters the brain, thereby increasing the content of dopamine in the brain and reducing its peripheral adverse reactions. The dosage ratio of benserazide hydrochloride and levodopa in Madopa is 1:4. [0003] The chemical name o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C241/04C07C243/34
CPCC07C241/04C07C243/34
Inventor 栗增翟其松赵鸿斐何先亮黄鲁宁陶安平安建国顾虹
Owner SHANGHAI SYNCORES TECH INC