ChemicalBook CAS DataBase List 2-Bromo-7-iodofluorene

2-Bromo-7-iodofluorene synthesis

13synthesis methods

Product Name:2-Bromo-7-iodofluorene
CAS Number:123348-27-6
Molecular formula:C13H8BrI
Molecular Weight:371.01

1133-80-8

123348-27-6

Example 7 Synthesis of 2-bromo-7-iodofluorene: 2-bromofluorene (12.61 g, 50 mmol), acetic acid (125 mL), water (9 mL), concentrated sulfuric acid (4 mL), iodine (5.1 g, 20.1 mmol), and iodic acid (2.2 g, 12.5 mmol) were mixed and heated to react for 2 hr at 80-90 °C. After completion of the reaction, the mixture was cooled and filtered. The resulting solid was washed sequentially with acetic acid (100 mL) and water (500 mL) to afford the target product 2-bromo-7-iodofluorene 14.7 g in 79% yield and melting point 179-185 °C. The product was analyzed by mass spectrometry. The results of mass spectrometry analysis (m/z): 418 (M + diiodo), 370, 372 (M + iodobromo), 322, 324, 326 (M + dibromo).

1133-80-8 Synthesis

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Yield:123348-27-6 98%

Reaction Conditions:

with potassium iodate;sulfuric acid;iodine;acetic acid in water at 80; for 12 h;Inert atmosphere;

Steps:

7 Example 7, Synthesis of 2-bromo-7-iodo-9H-fluorene (8)

2-bromoindole (2.44 g, 10 mmol), iodine (1.1 g, 4.5 mmol) and potassium iodate (0.65 g, 3 mmol) were dissolved in a mixed solvent (45 ml of glacial acetic acid, 5 ml of water and 2 ml of sulfuric acid). Under nitrogen protection, the reaction system was heated to 80 ° C for 12 h. After the reaction was completed, the reaction system was slowly cooled to room temperature, extracted with 10 ml of dichloromethane, and washed with water until neutral. The organic layer was dried over anhydrous sodium sulfate and filtered.The filtrate is recovered under reduced pressure,Residue column chromatography gave a white solid 3.63 g, yield 98%.

References:

CN109678686,2019,A Location in patent:Paragraph 0071-0073

1133-80-8 Synthesis

1133-80-8
351 suppliers
$6.00/5g