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Preparation method of hydroxycamptothecine

A technology of hydroxycamptothecin and camptothecin, which is applied in the field of preparation of hydroxycamptothecin, can solve the problems of low safety factor, long time-consuming, inconvenient reaction operation, etc., achieve high total yield, simple experimental operation, increase light The effect of chemical reaction conversion rate

Inactive Publication Date: 2018-11-06
SICHUAN AGRI UNIV
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Problems solved by technology

[0004] The purpose of the present invention is to improve the quinoline epoxidation method of chemical semi-synthesis of hydroxycamptothecin, solve the problems of time-consuming, low safety factor, and inconvenient reaction operation in the prior art, and establish a convenient, efficient, and environmentally friendly new method

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  • Preparation method of hydroxycamptothecine
  • Preparation method of hydroxycamptothecine
  • Preparation method of hydroxycamptothecine

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Embodiment Construction

[0024] The specific technical solutions of the present invention are described in conjunction with the examples.

[0025] The preparation method of hydroxycamptothecin comprises the following steps:

[0026] (1) N-oxidation reaction

[0027] Accurately weigh an appropriate amount of camptothecin and place it in a round bottom flask. Heating in a water bath, at 30-45°C, add an acid solvent, stir for 10 minutes, and dissolve camptothecin. Raise the temperature to 60-70°C at a constant speed, add the oxidizing agent sodium perborate, continue to stir and condense to reflux. The temperature rises and the reaction continues. After the reaction was completed, the heating was stopped, and it was naturally cooled to room temperature. The reaction liquid was concentrated under reduced pressure, a large amount of ice water was added to the concentrated liquid, and the crystallization occurred upon standing. After the crystals are completely precipitated, filter, wash with a small a...

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Abstract

The invention belongs to the technical field of synthetic drugs, and particularly relates to a preparation method of hydroxycamptothecine. An acid solvent dissolves camptothecin, an oxidizing agent sodium perborate is added, the reaction liquid is subjected to vacuum concentration after a constant temperature reaction is completed, ice water is added till a crystal is completely separated out, filtration, washing and drying are conducted, and 1-deoxycamptothecine is obtained; dioxane, acetonitrile, water and concentrated sulfuric acid are added into 1-deoxycamptothecine to be dissolved and stirred, the mixture is illuminated with an ultraviolet high pressure mercury lamp, and the ice water is condensed and flows back; vacuum concentration is conducted, the ice water is added till the crystal is completely separated out, filtration, washing and drying are conducted, and a crude product is obtained; and the crude product is purified. The preparation method of hydroxycamptothecine is simple to operate, safe and economic, green and environmentally friendly, and high in total yield.

Description

technical field [0001] The invention belongs to the technical field of synthetic medicines, and in particular relates to a preparation method of hydroxycamptothecin. Background technique [0002] 10-Hydroxycamptothecin (HCPT) is a ten-hydroxylated derivative of camptothecin isolated from the fruit and leaves of Camptotheca acuminata (Camptotheca acuminata). It is an important intermediate of camptothecin anticancer drugs, so finding and developing the preparation method of HCPT is one of the important directions of research and development of camptothecin anticancer drugs. At present, there are four methods for preparing HCPT: direct extraction method, biotransformation method, chemical total synthesis method, and chemical semi-synthesis method. In 2017, Cen Ye et al. used ultrasonic-microwave co-extraction of HCPT in magma fruit, with an average extraction rate of 4.61%. This method consumes a large amount of solvent, the extraction process is complicated, and the yield i...

Claims

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Application Information

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IPC IPC(8): C07D491/22
CPCC07D491/22
Inventor 蒲祥胡月高湖川张利邹平黄乾明罗应刚张程瑞
Owner SICHUAN AGRI UNIV
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