1-iododibenzo[b,d]furan synthesis
- Product Name:1-iododibenzo[b,d]furan
- CAS Number:857784-97-5
- Molecular formula:C12H7IO
- Molecular Weight:294.09
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Yield:857784-97-5 44%
Reaction Conditions:
Stage #1: 1-aminodibenzofuranwith hydrogenchloride;sodium nitrite at -10 - -5; for 0.5 h;
Stage #2: with potassium iodide at 0 - 25; for 8 h;
Steps:
1.S3; 2.S3
The product 1-aminodibenzofuran obtained in the step S2 was placed in a 100 mL round bottom flask.Then add 29.9mL of 4mol/L hydrochloric acid to make the system strong acid, and cool down to -10 °C.Add sodium nitrite solution (2.26g, 0.033mol), and control the temperature to -5 °C.After stirring for 30 min, add KI solution (9 g, 0.055 mol), and control temperature is less than 0 °C.Then, the reaction was carried out at 25 ° C for 8 h, and after completion of the reaction, the solid was filtered, and the solid was dissolved with dimethyl ether (40 mL), and the insoluble solid was filtered, and the organic phase of the filtrate was washed twice with aqueous sodium thiosulfate solution.Wash once, concentrate the organic phase to 10 mL, add petroleum ether (4 mL) and filterGet the crude,Add petroleum ether (4mL) to the crude product to dissolve and crystallize.White solid product1-iododibenzofuran4.0g,The yield of the product was 44%.The purity is 99%.
References:
CN110041295,2019,A Location in patent:Paragraph 0022; 0026; 0027; 0031
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