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Synthetic method of ibandronate

A technology of sodium ibandronate and synthesis method, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, drug combinations, etc., can solve problems such as low total yield and low yield, and achieve The effect of low production cost, high product yield and simple operation process

Inactive Publication Date: 2008-10-08
HANDE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main shortcoming of this technical scheme is that a large amount of waste water containing DMF is produced in the first step reaction scheme, and the yield is relatively low, only about 52.7%; %

Method used

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  • Synthetic method of ibandronate
  • Synthetic method of ibandronate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1, step one:

[0031] Raw material name Mass (g) Molecular mass Molar mass Molar ratio

[0032] 3-Methylaminopropionitrile (>98%) 85.8 84.1 1.0 1.0

[0033] 1-Bromopentane (>98%) 169.5 151 1.1 1.1

[0034] NaOH (>96%) 50.0 40 1.2 1.2

[0035] Tetrabutylammonium iodide (>99%) 3.7 369 0.01 0.01

[0036] Water 50.0 18 2.67 2.67

[0037] Toluene 216.5 (250ml) 92.14 2.35 2.35

[0038] 1. Add NaOH aqueous solution, 50ml (43.3g) toluene, tetrabutylammonium iodide, and 3-methylaminopropionitrile into a 500ml three-neck flask, install a general-purpose mercury thermometer, and stir mechanically, which is a common mechanical stirrer in the laboratory , water bath, stir for half an hour, and mix well;

[0039] 2. Maintain the temperature at 45°C and add 1-bromopentane dropwise, use a dropping funnel for two hours, stir at 45°C for 7 hours, use Shimadzu gas chromatography, model GC-14C, monitor until the end of the reaction;

[0040] 3. Add 200ml of water to disso...

Embodiment 2

[0077] Embodiment 2, step one:

[0078] Raw material name Mass (g) Molecular mass Molar mass Molar ratio

[0079] 3-Methylaminopropionitrile (>98%) 84.1 84.1 0.98 1.0

[0080] 1-Bromopentane (>98%) 160.0 151 1.04 1.06

[0081] NaOH (>96%) 44.0 40 1.06 1.08

[0082] Tetrabutylammonium iodide (>99%) 7.4 369 0.02 0.02

[0083] Water 44.0 18 2.67 2.72

[0084] Toluene 217 (250ml) 92.14 1.88 1.92

[0085]1. Add NaOH aqueous solution, 50ml toluene, tetrabutylamine iodide, and 3-methylaminopropionitrile into a three-necked flask, install a thermometer, stir mechanically, and stir in a water bath for half an hour, and mix well;

[0086] 2. Maintain the temperature at 25°C and add 1-bromopentane dropwise for two hours, stir at 25°C for 7 hours, and monitor by gas chromatography until the reaction is complete;

[0087] 3. Add 200ml of water to dissolve the solid and separate the liquid;

[0088] 4. The lower layer was extracted twice with 100ml×2 toluene, the organic phases were ...

Embodiment 3

[0124] Embodiment 3, step one:

[0125] Raw material name Mass (g) Molecular mass Molar mass Molar ratio

[0126] 3-Methylaminopropionitrile (>98%) 42.1 84.1 0.50 1

[0127] Pentyl bromide (>98%) 80.0 151 0.53 1.06

[0128] NaOH (>96%) 20.8 40 0.5 1

[0129] Tetrabutylammonium iodide (>99%) 3.7 369 0.01 0.02

[0130] Water 18.0 18 1.0 2

[0131] Toluene 104 (120ml) 92.14

[0132] 1. Add 50% NaOH aqueous solution, 20ml toluene, tetrabutylammonium iodide, and 3-methylaminopropionitrile into a 250ml three-necked flask, install a general-purpose mercury thermometer, magnetically stir, and stir in a 25-degree water bath for half an hour, and mix well.

[0133] 2. Add bromide pentane dropwise at 25°C, finish dropping in two hours, stir for 15 hours, and monitor by gas chromatography until the peak of the raw material disappears.

[0134] 3. Add 100ml of water to dissolve the solid and separate the liquid.

[0135] 4. The lower layer was extracted with 100ml of toluene, and th...

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Abstract

The invention discloses a method to synthesize ibandronate, aiming to simplify process and improve yield. The method includes the following steps: 1, producing crude 3-(N-methyl-N-n-amyl-amine)propionitrile liquid; 2, producing 3-(N-methyl-N-n-amyl-amine)propionic acid hydrochloride; 3, producing white crude ibandronate. Compared with the prior art, the method has less procedure and simple after-process and effectively improves total yield. Therefore, the method has high yield and low cost, and the operation is simple, safe and convenient for industrial production.

Description

technical field [0001] The invention relates to a preparation method of medicine, in particular to a synthesis process of ibandronic acid sodium. Background technique [0002] Primary osteoporosis, referred to as osteoporosis, is a common disease of postmenopausal women and the elderly, characterized by bone loss and destruction of normal bone microstructure, increased bone fragility, and a systemic systemic disease that easily leads to fractures. disease. As the population ages, the incidence of osteoporosis gradually increases. my country has a large population base and is about to enter an aging society. The harm of osteoporosis is becoming more and more significant. Osteoporotic fractures, in particular, are common in the vertebral body, hip and wrist, and will inevitably cause huge economic and social burdens. Therefore, the task of osteoporosis prevention and treatment is urgent and arduous. [0003] Currently, there are two types of drugs that are clinically used t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38A61P19/10
Inventor 李凡峰
Owner HANDE PHARMA
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