Method for producing pregnenolone acetic ester and 16-dehydropregnenolone acetate by utilizing infrared heating ring opening

A dienolone acetate, far-infrared technology, applied in steroids, organic chemistry and other directions, can solve the problems of prolonged production cycle, increased safety risks, and high heating temperature of heat transfer oil, to ensure product qualification rate, electric heating The effect of high conversion efficiency and precise temperature control

Inactive Publication Date: 2011-10-19
湖北民生生物医药有限公司
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  • Summary
  • Abstract
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Problems solved by technology

When using traditional equipment, it is difficult to control the reaction temperature, pressure, and time during the production process. A little carelessness can easily lead to failure or incomplete reaction of the ring-opening cracking reaction, resulting in reduced yield and unqualified quality.
[0006] 2. The material in the kettle undergoes a high-temperature and high-pressure reaction. The reaction temperature is 210°C, the pressure is 0.6Mpa, the heating temperature of the heat transfer oil is high, and the electric heating tube is used for heating. On

Method used

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Examples

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Embodiment Construction

[0018] The method of producing dienolone acetate through silicon carbide far-infrared heating ring opening, throwing 160kg of diosgenin, adding 88kg of glacial acetic acid, 252kg of acetic anhydride, and 96kg of mother liquor. The infrared heating control cabinet automatically controls the switch to carry out the ring-opening cracking reaction. When the internal temperature rises to 196°C and the internal pressure reaches 0.44MPa, the meter automatically cuts off the power and counts. The ring-opening cracking reaction was carried out for 60 minutes, and finally the internal temperature reached 208° C. and the ring-opening was completed under a pressure of 0.58 MPa. Press into the oxidation hydrolysis tank prepared with 90kg base acid, and start to lower the temperature. When the temperature in the tank drops to 10-12°C, close the brine, and immediately add the oxidant to the oxidation tank to carry out the oxidation reaction. When the temperature rose to 98°C, the reaction w...

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PUM

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Abstract

A method for producing pregnenolone acetic ester and 16-dehydropregnenolone acetate by utilizing infrared heating ring opening comprises the steps of ring-opening cracking, extraction and refining, wherein infrared heating is carried out on a reaction kettle during ring-opening cracking process. In the invention, as a silicon carbide far infrared heating and radiation heating device and a tank body are assembled together, the reaction kettle is heated by controlling the voltage and current of a heating device, so that temperature and voltage can be automatically controlled, power can be automatically adjusted and randomly set, the temperature control is precise, heat buffer is small, personal errors are reduced, the stability of infrared heating ring-opening reaction is ensured, and further the reaction is more sufficient.

Description

technical field [0001] The invention belongs to the technical field of clean production of steroid hormone drug intermediates, and in particular relates to a process for producing mono- and dienolone acetates through silicon carbide far-infrared heating and ring-opening. Background technique [0002] Dienolone acetate (referred to as diene) Chemical name: 5.16-pregnadiene-3β-ol-20-one acetate, molecular formula C 23 h 32 o 3 , which has the parent nucleus of cyclopentane-perhydrophenanthrene, which is a typical steroid compound. Diene is an important intermediate in the synthesis of various steroid hormone drugs, which can be used as raw materials to produce progesterone drugs (progesterone, medroxyprogesterone, progesterone caproate), adrenal cortex hormone drugs (such as hydrocortisone , prednisone, betamethasone,) sex hormones and anabolic hormone drugs (methyl testosterone, medroxyprogesterone, anadrol, stanozolol), etc. [0003] The ring-opening cleavage reaction is...

Claims

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Application Information

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IPC IPC(8): C07J13/00
Inventor 陈孝华
Owner 湖北民生生物医药有限公司
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