2,7-Dibromo-4,5-Diazafluoren-9-one synthesis
- Product Name:2,7-Dibromo-4,5-Diazafluoren-9-one
- CAS Number:77213-41-3
- Molecular formula:C11H4Br2N2O
- Molecular Weight:339.97
100125-12-0
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Yield:77213-41-3 52%
Reaction Conditions:
Stage #1: 3,8-dibromo-1,10-phenathrolinewith potassium hydroxide in water; for 1 h;Reflux;
Stage #2: with potassium permanganate in water; for 2 h;Reflux;
Steps:
1 Synthesis of Intermediate 1-1:
Dissolve 0.1 mol of 3,8-dibromophenanthroline and 0.3 mol of KOH in 1500 ml of water and reflux for 1 h, and gradually add 1 L of 0.03 mol of KMnO4 hot saturated aqueous solution.The reaction solution was refluxed for 2 hours. After the reaction was completed, it was filtered while it was hot. The filtrate was cooled to room temperature. A large number of needle-like crystals were precipitated. After filtration, the filtrate was extracted 3 times with chloroform. The organic phases were combined. Rotary evaporation to remove the solvent to obtain a yellow solid, and finally intermediate 1-1 (yield: 52%).
References:
CN111518126,2020,A Location in patent:Paragraph 0156; 0157; 0158
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