ChemicalBook CAS DataBase List Dibenzofuran, 1-nitro-

Dibenzofuran, 1-nitro- synthesis

12synthesis methods

Product Name:Dibenzofuran, 1-nitro-
CAS Number:87812-99-5
Molecular formula:C12H7NO3
Molecular Weight:213.19

99-65-0 Synthesis

99-65-0
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533-58-4 Synthesis

533-58-4
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87812-99-5
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Yield: 76%

Reaction Conditions:

with pyridine;copper(l) iodide;potassium tert-butylate in toluene at 110 - 115; for 5 h;Inert atmosphere;

Steps:

7.1 (1) compound 28, compound 29
In a 500 ml three-necked bottle equipped with a thermometer and a condenser, 200 ml of toluene, 46 g of t-BuOK were sequentially added, and the air in the reaction bottle was replaced with nitrogen, and 7.8 g of CuI was added under nitrogen protection.Stir for 1 h, then add 23 g of 50 ml of pyridine solution of 1,3-dinitrobenzene, the solution turns into a red turbid solution, continue to add 30 g of intermediate 28, and heat to (110-115 ° C) under reflux.After 5h, samples were taken and tested. The reaction was stopped when the reaction of the raw materials was complete. The temperature was lowered to room temperature for post-treatment. The reaction solution was filtered, and a 1M hydrochloric acid solution was added to adjust the pH to be neutral. The aqueous phase was extracted with 100 ml of toluene. The organic phases were combined, washed once with saturated brine, dried over anhydrous Na 2 SO 4 for 1 h, filtered to remove the desiccant, and concentrated to obtain intermediate 29 after purification through a silica gel column. Intermediate 29 was 22.1 g of a pale yellow solid with a yield of 76%.

References:

Xi'an Ruilian New Materials Co., Ltd.;Sun Jun;Zhang Hongke;Liu Kaipeng;Wang Xiaowei;Liu Qianfeng;Gao Renxiao CN108047235, 2019, B Location in patent:Paragraph 0231; 0234-0237