Synthetic method for hormone intermediate androsten-17alpha-methyl-17beta-ol-3-one

A synthetic method and intermediate technology, applied in the field of organic synthesis, can solve the problems of increasing the risk factor of the reaction process, large environmental pollution, and complicated synthesis process, and achieve the goals of shortening the reaction time, increasing the risk factor, and improving the reaction yield Effect

Inactive Publication Date: 2018-07-03
CHENGDU QIESITE TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the existing synthetic methods use chromium oxide and concentrated sulfuric acid as reactants. Because chromium oxide is more polluting to the environment, concentrated sulfuric acid will increase the risk factor of the reaction process as a reactant, and the whole synthesis process is more complicated. Therefore, it is necessary to propose a A new synthetic method

Method used

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  • Synthetic method for hormone intermediate androsten-17alpha-methyl-17beta-ol-3-one

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The synthetic method of hormone intermediate androst-17α-methyl-17β-alcohol-3-one comprises the following steps:

[0018] A. Add 2mol of androsta-17-α-methyl-2β, 3β, 17β-triol-4-amino in the reaction vessel, 800ml of diphenyl ether solution with a mass fraction of 30%, and control the temperature of the solution to 10°C , control the stirring speed at 170rpm, react for 60min, add 1.6L of potassium nitrate solution with a mass fraction of 15%, and continue to react for 30min;

[0019] B, the mass fraction that adds 4mol is 35% propyl valerate solution, raises solution temperature to 40 ℃, divides the tetrakis (phosphorous trichloride) nickel powder that adds 3 mol, continues reaction 80min, adds mass fraction is Washing with 40% cyclohexane solution, washing with 10% sodium bromide solution in 900ml mass fraction, washing with 50% methyl propyl ether solution, and recrystallization in 80% cyclopentanol solution , dehydrated with anhydrous calcium sulfate dehydrating age...

Embodiment 2

[0021] The synthetic method of hormone intermediate androst-17α-methyl-17β-alcohol-3-one comprises the following steps:

[0022] A. Add 2mol of androsta-17-α-methyl-2β, 3β, 17β-triol-4-amino in the reaction vessel, 800ml of diphenyl ether solution with a mass fraction of 33%, and control the temperature of the solution to 12°C , control the stirring speed at 190rpm, react for 70min, add 1.6L mass fraction of 17% potassium nitrate solution, continue to react for 40min;

[0023] B. Add 5mol mass fraction of 39% propyl valerate solution, increase the solution temperature to 42°C, add 3.5mol tetrakis (phosphorus trichloride) nickel powder in 5 times, continue the reaction for 90min, add a mass fraction of 43 % cyclohexane solution washing, 900ml mass fraction is 13% sodium bromide solution washing, mass fraction is 53% methyl propyl ether solution washing, and mass fraction is 83% cyclopentanol solution for recrystallization, Dehydration with anhydrous potassium carbonate dehydra...

Embodiment 3

[0025] The synthetic method of hormone intermediate androst-17α-methyl-17β-alcohol-3-one comprises the following steps:

[0026] A, add 2mol androst-17-α-methyl-2β in reaction vessel, 3β, 17β-triol-4-amino, 800ml mass fraction is 37% diphenyl ether solution, control solution temperature to 15 ℃, Control the stirring speed to 210rpm, react for 80min, add 1.6L potassium nitrate solution with a mass fraction of 22%, and continue to react for 50min;

[0027] B. Add propyl valerate solution with a mass fraction of 41%, increase the solution temperature to 45°C, add 4 mol tetrakis(phosphorus trichloride) nickel powder in 7 times, continue the reaction for 100min, and add a mass fraction of 46% Cyclohexane solution washing, 900ml mass fraction of 17% sodium bromide solution washing, mass fraction of 56% methyl propyl ether solution washing, recrystallization in the mass fraction of 87% cyclopentanol solution, di Phosphorus dehydrating agent dehydration, the finished product androst-...

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Abstract

The invention discloses a synthetic method for the hormone intermediate androsten-17alpha-methyl-17beta-ol-3-one. The synthetic method comprises the following steps: adding androsten-17-alpha-methyl-2beta,3beta,17beta-triol-4-amine and a diphenyl ether solution into a reaction vessel, controlling solution temperature and a stirring speed, adding a potassium nitrate solution and continuing a reaction; and adding a propyl valerate solution, raising solution temperature, adding tetrakis(phosphorus trichloride)nickel powder in batches, continuing the reaction, carrying out washing with a cyclohexane solution, then carrying out washing with a sodium bromide solution, then carrying out washing with a methyl propyl ether solution, carrying out recrystallization in a cyclopentanol solution, and then carrying out dehydration with a dehydrating agent so as to obtain the finished androsten-17alpha-methyl-17beta-ol-3-one.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate, belonging to the field of organic synthesis, in particular to a synthesis method of a hormone intermediate androsta-17α-methyl-17β-ol-3-one. Background technique [0002] Androst-17α-methyl-17β-ol-3-one, as a hormone intermediate, is mainly used in the synthesis of dehydromethyltestosterone. The protein synthesis effect of dehydromethyltestosterone is similar to that of testosterone, but its protein assimilation effect is stronger than that of androgen, and its masculinization effect is weaker. It can make nitrogen, potassium, sodium, calcium, phosphorus, and chlorine retention, increase weight, and promote Osteogenesis and body growth and development. For osteoporosis and comminuted fractures caused by cortisone treatment, relief of menopausal back pain, recovery from chronic wasting disease and surgery, excessive loss of nitrogen in severe burns, promotion of premature i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J1/00
CPCC07J1/0037
Inventor 彭飞
Owner CHENGDU QIESITE TECH CO LTD
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