Preparation process of standard products of morphine base and heroin base

A technology for heroin and standard products, which is applied in the field of preparation of heroin base and morphine base standard products, can solve the problems of a large number of high-purity reagents and high-priced equipment investment, and achieve the effect of reducing costs

Inactive Publication Date: 2015-06-10
YUNNAN UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method requires expensive equipment investment and a lar

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  • Preparation process of standard products of morphine base and heroin base
  • Preparation process of standard products of morphine base and heroin base

Examples

Experimental program
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Embodiment 1

[0025] Embodiment 1: Preparation of standard substances of heroin base and morphine base

[0026] Morphine preparation:

[0027] Acid hydrolysis: 50 grams of crude heroin for experiment, with 3mol L -1 300ml of hydrochloric acid for deacetylation reaction. After filtering the resulting solution, heat at 80°C for 60 minutes. After cooling, adjust the pH to neutral with solid sodium hydroxide (precipitation occurs), and then use saturated aqueous sodium carbonate to adjust the pH to 9 (until sodium carbonate is added dropwise). Precipitation occurs again), and the precipitate was left for 5 hours, suction filtered, washed with water, and the precipitate was dried by infrared to obtain 35 g of crude morphine, with a conversion rate of 70%.

[0028] Refining of morphine: The crude morphine was ultrasonically washed with 10 times the amount of diethyl ether, filtered 3 times, dried, purified by silica gel chromatography, and recrystallized from methanol 4 times. Get 17.6 grams of m...

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Abstract

The invention discloses a preparation process of standard products of morphine base and heroin base. The preparation process comprises the following steps: (1) carrying out methanol extraction and acid hydrolysis on a heroin sample obtained during drug control, so as to obtain a morphine crude product; (2) purifying by virtue of silica gel chromatography preparation column; (3) carrying out methanol recrystallization to obtain a morphine standard product; (4) carrying out acetylation on morphine, so as to obtain a heroin sample; and (5) recrystallizing concentrated liquid obtained in the step (4), so as to obtain a heroin base standard product, wherein the detection result of gas chromatography mass spectrometry shows that the purity of morphine base is more than or equal to 97.8% and the purity of heroin is more than or equal to 98.4%. According to a project design, all technique processes are carried out at normal temperature and normal pressure, the operation is simple, safe and environmentally friendly, and the preparation cost is low.

Description

technical field [0001] The invention relates to a process for preparing heroin base and morphine base standard products. The technical problem to be solved by the present invention is to provide a method for preparing heroin base and morphine base standard products with mild reaction conditions, high yield, low cost, green and safe. Background technique [0002] In the morphine alkaloid drug, derived from the natural product opium poppy (scientific name: Papaver somniferum L. ), morphine and codeine can be extracted from poppy, and their acetylated products 3-monoacetylated morphine, 6-monoacetylated morphine, 3,6-diacetylated morphine (heroin), acetylated Codeine, morphine is similar to the molecular structure of codeine, the 3-OH on the molecule is morphine, and the 3-OCH on the molecule 3 It is codeine, and the acetylation of 6-OH on the codeine molecule is acetylated codeine, such as figure 1 shown. It is difficult for a single pure chemical substance to exist indep...

Claims

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Application Information

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IPC IPC(8): C07D489/02
CPCC07D489/02
Inventor 李虹刑豫明段德良王家强赵文嵩焦德强
Owner YUNNAN UNIV
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