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photoreaction device

A technology of photoreaction and reaction vessel, which is applied in the field of photoreaction equipment, can solve the problems such as the need for improvement of the photoreaction device, and achieve the effects of simple operation, strong controllability and good light quality.

Active Publication Date: 2017-03-01
HUBEI BIO PHARMA IND TECHCAL INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, current photoreaction equipment still needs to be improved

Method used

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Examples

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Embodiment 1

[0065] In this embodiment, utilize light reaction equipment to synthesize hypericin through the following steps:

[0066] (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 2O 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;

[0067] (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, and stir...

Embodiment 2

[0072] In this example, 2-bromo-2-(2-fluorophenyl)-1-cyclopropylethanone was synthesized by the following steps using photoreaction equipment:

[0073] 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.

[0074] 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 formula: H / R2 is ...

Embodiment 3

[0077] In this example, the novel oleanolic acid derivatives were synthesized through the following steps using photoreaction equipment:

[0078] (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;

[0079] (2) Add dry CH successively to the r...

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Abstract

The invention discloses a photoreaction device, and provides photoreaction equipment. The photoreaction equipment comprises a reaction container and a light source according to an embodiment of the invention. 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 photoreaction equipment has the advantages that the photoreaction equipment is easy and convenient to operate and high in controllability and illumination quality, or photoreaction can be completely guaranteed.

Description

technical field [0001] The invention relates to the field of chemical industry. In particular, the invention relates to photoreaction devices. 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 photoreaction devices still need to be improved. 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 photoreaction device, which is easy to operate, strong in controllability, better in light quality or more completely guarantees the progress of the photochemical reaction. [0005] It sho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/12
Inventor 王学海许勇杨仲文张毅黄璐张守波熊传超黄文杰
Owner HUBEI BIO PHARMA IND TECHCAL INST
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