Gas separation flow system and gas separation flow method for photochemical synthesis of 9-beta,10-alpha-dehydroprogesterone ketal

A photochemical synthesis, ketone ketal technology, applied in chemical instruments and methods, organic chemistry, steroids, etc., can solve the problems of gas expansion, large pressure drop, and reduced light exposure time, and achieve increased pipe diameter and system Effects of flux, increased conversion and yield, and reduced boundary layer thickness

Active Publication Date: 2020-03-13
SHANDONG TSINGCHUANG CHEMICALSCO LTD +2
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, for photochemical reactions such as the synthesis of 9-β, 10-α-dehydroprogesterone ketal, etc., after multiple photochemical devices, the total length of the reaction tube is more than 50m or even 100m, and the pressure drop in the tube is relatively large; even if the gas If it does not participate in the reaction, the two-phase flow formed at the initial stage will also experience gas expansion in the rear section of the reaction tube, causing the fusion of adjacent liquid columns and the acceleration of the total flow rate, resulting in the formation of local homogeneous flow and the shortening of the reactant exposure time. A sharp decrease, affecting the conversion rate and yield of photochemical reactions

Method used

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  • Gas separation flow system and gas separation flow method for photochemical synthesis of 9-beta,10-alpha-dehydroprogesterone ketal
  • Gas separation flow system and gas separation flow method for photochemical synthesis of 9-beta,10-alpha-dehydroprogesterone ketal
  • Gas separation flow system and gas separation flow method for photochemical synthesis of 9-beta,10-alpha-dehydroprogesterone ketal

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Effect test

Embodiment 1

[0051] A gas-separated flow system for two-step photochemical synthesis of 9-β, 10-α-dehydroprogesterone ketal, which includes a gas-liquid micro-mixing unit, 2 sets of photochemical reaction devices with built-in light sources and a back pressure valve, that is, gas-liquid The micro-mixing unit and the first photochemical reaction device (comprising the first tube reactor, the first tube light source and the first cold trap) and the second photochemical reaction device (comprising the second tube reactor, the second light source and the second cold trap) trap), and the outlet of the reactor was connected to a back pressure valve.

[0052] The inner diameter of the main pipe in the gas-liquid micro-mixing unit is 1 mm, and the inner diameter of the side pipe is 0.1 mm; the first tubular reactor is a polytetrafluoroethylene tube with an inner diameter of 1 mm and an outer diameter of 2 mm; the second tubular reactor is a polytetrafluoroethylene tube with an inner diameter of 2m...

Embodiment 2

[0059] A gas-separated flow system for the one-step photochemical synthesis of 9-β, 10-α-dehydroprogesterone ketal, which consists of a gas-liquid micro-mixing unit, 3 sets of photochemical reaction devices with built-in light sources and a back pressure valve, that is, gas-liquid The micro-mixing unit and the first photochemical reaction device (comprising the first tube reactor, the first light source and the first cold trap), the second photochemical reaction device (comprising the second tube reactor, the second light source and the second cold trap ) and a third photochemical reaction device (including a third tubular reactor, a third light source and a third cold trap), and the outlet of the reactor is connected to a back pressure valve.

[0060] The inner diameter of the main pipe in the gas-liquid micro-mixing unit is 2mm, and the inner diameter of the side pipe is 1mm; the first, second and third tubular reactors are all perfluoroethylene propylene copolymer tubes with...

Embodiment 3

[0067]A gas-separated flow system for the two-step photochemical synthesis of 9-β, 10-α-dehydroprogesterone ketal, which includes a gas-liquid micro-mixing unit, 4 sets of photochemical reaction devices with built-in light sources and a back pressure valve, that is, gas-liquid The micro-mixing unit and the first photochemical reaction device (comprising the first tube reactor, the first light source and the first cold trap), the second photochemical reaction device (comprising the second tube reactor, the second light source and the second cold trap ), the third photochemical reaction device (comprising the third tube reactor, the third light source and the third cold trap) and the fourth photochemical reaction device (comprising the fourth tube reactor, the fourth light source and the fourth cold trap) , the outlet of the reactor is connected to a back pressure valve.

[0068] The gas-liquid micro-mixing unit is that the inner diameter of the main pipe is 2mm, and the inner d...

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Abstract

The invention relates to a gas separation flow system and a gas separation flow method for photochemical synthesis of 9-beta,10-alpha-dehydroprogesterone ketal. The method is characterized in that 9-beta,10-alpha-dehydroprogesterone ketal is synthesized in one step or two steps by utilizing ultraviolet light with different wave bands, a raw material 9-alpha,10-beta-dehydroprogesterone ketal reaction solution is separated by gas doing not participate in a reaction, the internal disturbance of the reaction solution is enhanced, and the retention time of the reaction solution in a tubular reactoris ensured to be consistent. The method has the advantages of being continuous, stable, high in light energy utilization rate, low in production cost, easy and convenient to operate and controllablein process, and has huge prospect in the industrial production of 9-beta,10-alpha-dehydroprogesterone ketal through photochemical synthesis.

Description

technical field [0001] The invention belongs to the field of organic photochemical synthesis, in particular to a gas separation flow system and method for photochemically synthesizing 9-β, 10-α-dehydroprogesterone ketal. Background technique [0002] Dydrogesterone is a progestogen drug used for a variety of indications, including threatened or recurrent pregnancy loss, dysfunctional bleeding, and disorders caused by endogenous progesterone insufficiency. Dydrogesterone was first studied in the 1950s, and its high-efficiency synthesis method has been closely watched, especially the method of using progesterone as a raw material has become the focus of continuous attention of researchers [Pharmaceutical Manufacturing Encyclopedia, 3rd Edition.WilliamAndrew Publishing. 1411.; Olbrich, M., Weigl, K., Kahler, E, Mihara, K., Xenobiotica. 2016, 46, 868]. [0003] In the synthetic route of progesterone, the step of photochemically synthesizing 9-β, 10-α-dehydroprogesterone ketal w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J21/00
CPCC07J21/005
Inventor 陈桂光杜乐申春符绍东米嘉李阳李昊蔡保理孙保锁尹佳滨
Owner SHANDONG TSINGCHUANG CHEMICALSCO LTD
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