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ChemicalBook CAS DataBase List 3,4,9,10-Perylenetetracarboxylic dianhydride
128-69-8

3,4,9,10-Perylenetetracarboxylic dianhydride synthesis

8synthesis methods
-

Yield:128-69-8 175 g

Reaction Conditions:

Stage #1:3,4,9,10-perylene tetracarboxyxlic acid diimide with sulfuric acid at 220; for 2 h;
Stage #2: with potassium hydroxide in water at 90; for 1 h;Darkness;Inert atmosphere;Further stages;

Steps:

4 Example 4
In the reaction bottle, At room temperature, 3,4,9,10-decanetetracarboxylic acid diimide 200g Slowly added to concentrated sulfuric acid 700g (content 95%), After the addition, slowly increase the temperature to 220 ° C, Keep the temperature reaction for 2h, Then slowly drop to room temperature, A large amount of solids precipitated during the cooling process. Filter the reaction solution, Wash the filter cake with water to neutral, Drying the filter cake at 80 ° C to obtain crude 3,4,9,10-guanidine;The obtained crude product was all added to a mixed solution of 6000 mL of water and 140 g of potassium hydroxide (85% of content) in the dark, Under the protection of nitrogen, Slowly heat to 90 ° C, The reaction was stirred at room temperature for 1 h and then cooled to room temperature. There is a lot of solid precipitation, Vacuum filtration of the reaction solution, The filter cake was washed with 100 mL of water; Under nitrogen protection and protection from light, 60 g of potassium hydroxide (85% content) and 60 g of activated carbon were added to the filtrate. After stirring at room temperature for 30 min, 60 g of ferric chloride and 600 mL of water were added. Stir the reaction at room temperature for 30 min, Filter the reaction solution, 600 g of saturated hydrochloric acid solution was added to the filtrate. Heat to 80 ~ 90 ° C for 1 h, There are a lot of solids, After dropping to room temperature, the reaction solution was filtered. The filter cake was dried to obtain 175 g of 3,4,9,10-perylenetetracarboxylic dianhydride.

References:

Henan Wanliu Biological Technology Co., Ltd.;Yang Weixiao;Hou Yansheng CN108864153, 2018, A Location in patent:Paragraph 0028-0030

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