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photoreaction equipment

A photoreaction and equipment technology, applied in the chemical industry, can solve the problems to be improved, and achieve the effect of simple operation, strong controllability and convenient operation

Active Publication Date: 2017-02-22
HUBEI BIO PHARMA IND TECHCAL INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, current systems for preparing compounds still need to be improved

Method used

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Examples

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Effect test

Embodiment 1

[0067] In this example, hypericin was synthesized by the following steps using the system used to prepare the compound:

[0068] (1) Add 840 mg (3 mmol) of emodin and 50 mL of glacial acetic acid in a four-necked bottle, N 2 protection, add SnCl under stirring 2 2H 2 O 2.84g (12.6mmol), after warming up to reflux, slowly add 5mL of 48% hydrobromic acid dropwise (in 4 drops at intervals of 30min); after addition, continue to react for 2h (TLC tracking). Cool to room temperature, filter with suction, wash the filter cake with water until neutral, and dry to obtain 2672 mg of light yellow powder;

[0069] (2) Add the powder 2512mg (2mmol) that step (1) obtains in four-necked bottle successively, pyridine 10mL, FeSO 4 ·7H 2 O 820mg (0.295mmol), pyridine nitrogen oxide 1.25g (13.2mmol) and pyridine 1 mL, N 2 Protected from light and heated to reflux (100° C.) for 1.5 h (TLC tracking). Cool to room temperature, evaporate the organic solvent, add 200mL of 3% hydrochloric acid, ...

Embodiment 2

[0074] In this example, 2-bromo-2-(2-fluorophenyl)-1-cyclopropylethanone was synthesized by the following steps using the system used to prepare the compound:

[0075] In a 250mL three-necked round bottom flask equipped with a stirrer and a thermometer, add 10.0g (56.1mmol) of 2-(2-fluorophenyl)-1-cyclopropylethanone, 100mL of dichloromethane, dibromohydantoin (8.0 g, 28.0 mmol), benzoyl peroxide (0.5g), at room temperature, react 4h under the illumination of 15W sight light, then cool, concentrate and reclaim methanol, the residue is dissolved in dichloromethane, filters, and the filtrate Washed to neutral, anhydrous MgSO 4 Dry and concentrate under reduced pressure to constant weight to obtain light yellow oil.

[0076] The height of the liquid level limiter of the photoreaction equipment from the bottom of the reaction vessel is H, and the average distance between the light source and the vertical axis of the reaction vessel is R2, wherein H and R2 satisfy the relational f...

Embodiment 3

[0079] In this example, a novel oleanolic acid derivative was synthesized by the following steps using the system used to prepare the compound:

[0080] (1) Add 60mL of diethyl ether and 20ml of 40% KOH solution to the flask, add 6g of methylnitrosourea in batches under stirring at below 5°C; react for 10min, separate the ether layer to obtain CH 2 N 2 Diethyl ether solution, dried with KOH for later use. Add 110g (21.9mmol) of THF (20mL) solution into the reaction flask, add CH 2 N 2 Diethyl ether solution, after dropping, reacted to the end point (monitored by TLC). The solvent was evaporated, the residue was dried and CHCl was added 3 50ml and pyridine 30mL, add Ac 2 O 10mL, after addition, react at room temperature to the end. Water, 5% HCl solution, saturated NaHCO 3 Solution, water and saturated brine washing, anhydrous MgSO 4 dry. After distilling off the solvent, recrystallize with ethyl acetate to obtain white crystals;

[0081] (2) Add dry CH successively t...

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Abstract

The invention provides a system for preparing chemical compounds. The system for preparing the chemical compounds comprises photoreaction equipment and purification equipment according to an embodiment of the invention. The purification equipment is connected with the photoreaction equipment, the photoreaction equipment comprises a reaction container and a light source, a photoreaction space is defined in the reaction container, and the reaction container is made of transparent materials; the light source is arranged on the outside of the reaction container. The system for preparing the chemical compounds has the advantages that the system is easy and convenient to operate and high in controllability and illumination quality, or photochemical reaction can be completely guaranteed.

Description

technical field [0001] The invention relates to the field of chemical industry. In particular, the invention relates to systems for preparing compounds. Background technique [0002] Photochemical reaction refers to the chemical reaction process that occurs under the irradiation of an external light source, and is a reaction triggered by the absorption of photons by the molecules of a substance. In the field of chemistry and pharmaceutical chemical industry, the application of photochemical reaction is of great significance. [0003] However, current systems for preparing compounds leave room for improvement. Contents of the invention [0004] The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, an object of the present invention is to provide a system for preparing compounds, which is easy to operate, strong in controllability, better in light quality or more completely guarantees the progress of photochemical...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/12C07C50/36C07C46/00C07C45/63C07C49/567C07J63/00
Inventor 王学海许勇杨仲文张守波张毅黄璐熊传超黄文杰
Owner HUBEI BIO PHARMA IND TECHCAL INST
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