Recovering and reusing method of resolving agent quinine

A kind of resolving agent, separation technology

Inactive Publication Date: 2018-03-20
HANGZHOU XINBOSI BIOMEDICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the used quinine is directly discarded after the split in the patent, which not onl...

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  • Recovering and reusing method of resolving agent quinine

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Embodiment 1

[0019] recycling part

[0020] The crystallization mother liquor in the above reaction was placed in a 60°C water bath and concentrated under reduced pressure to about 120ml, then added 130ml of 1mol / L hydrochloric acid aqueous solution, and then 150ml of dichloromethane, stirred for 1 hour, and stood to separate layers. Add 80ml of 2mol / L sodium hydroxide aqueous solution to the upper aqueous phase, and measure pH=13.12 with a Mettler pH meter; add 250ml of dichloromethane, stir for 1 hour, and let stand to separate layers; collect the dichloromethane phase, and then use 200ml of dichloromethane Extract with methane, combine the dichloromethane phases, add 30 g of anhydrous sodium sulfate to dry, then place in a water bath at 40°C and concentrate to dryness. Add 200ml of ethanol to the concentrate, raise the temperature to reflux and stir for 1h, then cool down to -10°C and stir for 4h. After filtration, the filter cake was air-dried in an oven at 60° C. to dryness to obtain...

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Abstract

The invention relates to a recovering and reusing method of a resolving agent quinine for preparing a key intermediate S-1,2,3,4-tetrahydro-1-naphthoic acid of palonosetron hydrochloride. The recovering and reusing method comprises the following steps: taking a resolving and crystallizing mother solution of racemic 1,2,3,4-tetrahydronaphthoic acid as a raw material; acidifying and carrying out extracting separation; then alkalinizing and separating out an organic phase; finally, concentrating and recrystallizing to obtain quinine with qualified optical rotation, wherein the quinine can be usedfor resolving the 1,2,3,4-tetrahydronaphthoic acid again. According to the recovering and reusing method disclosed by the invention, by recovering and reusing the resolving agent quinine in reactingwaste solution generated by preparing an S-1,2,3,4-tetrahydro-1-naphthoic acid, the production cost is greatly reduced, discharge of a nitrogen-containing waste solution is reduced and environmental protection is benefited; in addition, the recovering and reusing method is simple in industrial operation and easy for industrialization realization.

Description

technical field [0001] The present invention relates to a kind of palonosetron hydrochloride key intermediate ( S )-1,2,3,4-tetrahydro-1-naphthoic acid recovery process, specifically relates to a resolution agent quinine recovery process method. Background technique [0002] Quinine (QN for short), also known as cinchona alkali, cinchona cream, molecular formula C20H24N2O2, relative molecular weight 324.42, CAS number: 130-95-0, IUPAC name: (R)-(6-methoxy Quinolin-4-yl)((2S,4S,8R)-8-vinylquinuclidin-2-yl)methanol, the structural formula is: [0003] [0004] Quinine is the earliest antimalarial drug discovered and used by humans, and it is also an important chiral catalyst widely used in the field of asymmetric catalysis of small organic molecules. It has recently been found to be effective in treating leg cramps and other muscle spasms. Because the difficulty and cost of artificially synthesizing quinine are all relatively high, so the extraction process of separating...

Claims

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Application Information

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IPC IPC(8): C07C51/487C07C61/39C07B57/00C07D453/02
CPCC07B57/00C07B2200/07C07C51/487C07D453/02C07C61/39
Inventor 陈德宝刘艳华
Owner HANGZHOU XINBOSI BIOMEDICAL CO LTD
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