ChemicalBook CAS DataBase List 5H-Pyrrolo[3,4-b]pyridine-5,7(6H)-dione

5H-Pyrrolo[3,4-b]pyridine-5,7(6H)-dione synthesis

9synthesis methods

Product Name:5H-Pyrrolo[3,4-b]pyridine-5,7(6H)-dione
CAS Number:4664-00-0
Molecular formula:C7H4N2O2
Molecular Weight:148.12

89-00-9

4664-00-0

General procedure for the synthesis of 2,3-pyridinedicarboximide from 2,3-pyridinedicarboxylic acid: 167 g of 2,3-pyridinedicarboxylic acid (1.0 mol) and 300 mL of concentrated ammonia (28%) were added to a 1000 mL three-necked flask, followed by refluxing and stirring for 6 hours at 140 °C. The reaction was carried out in a liquid mixture of 2,3-pyridinedicarboxylic acid (1.0 mol) and 300 mL of concentrated ammonia (28%). During the reaction, the liquid reaction mixture gradually changed to dark brown color. The progress of the reaction was monitored by thin layer chromatography (TLC) and after confirming the complete reaction of 2,3-pyridinedicarboxylic acid, the reaction mixture was cooled to room temperature. Under continuous stirring, the reaction mixture was slowly poured into 500 mL of cold water, and a large amount of gray solid precipitated immediately. The solid product was collected by filtration and the filter cake was washed with cold water and subsequently dried under vacuum at 60 °C overnight to give 125 g of gray powdery product in 84% yield.

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4664-00-0
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Yield:4664-00-0 84%

Reaction Conditions:

with ammonium hydroxide at 140; for 6 h;Reagent/catalyst;

Steps:

9 Preparation of pyrrolo[3,4-b]pyridine-5,7-dione
To 1000 ml three-necked flask were added 167 g of 2,3-pyridinedicarboxylic acid (1.0 mol) and 300 ml of concentrated aqueous ammonia (28%), followed by stirring under reflux for 6 hours at 140 °C, the liquid reaction mixture became dark brown, thin layer Analysis of the reaction was followed, when the starting material 2,3-pyridinedicarboxylic acid completion of the reaction, the reaction mixture was cooled to room temperature, under stirring, the reaction mixture was cooled as slowly pouredinto 500 ml of cold water, a large number of gray solid immediately precipitated, was filtered and the filter cake washed with coldwater and dried in vacuo overnight at 60 °C, to give a gray powder 125 g, yield 84%.

References:

Guo Feng;Guo, Feng CN102746294, 2016, B Location in patent:Paragraph 0077; 0078

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