ChemicalBook CAS DataBase List 2-Bromo-9,9'-spirobi[9H-fluorene]

2-Bromo-9,9'-spirobi[9H-fluorene] synthesis

13synthesis methods

Product Name:2-Bromo-9,9'-spirobi[9H-fluorene]
CAS Number:171408-76-7
Molecular formula:C25H15Br
Molecular Weight:395.29

Synthesis of 2-bromo-spirofluorene
2-bromo-9-hydroxy-9-(2-biphenyl)fluorene (2g) dissolved in 25 mL acetic acid (15 mol/L) containing hydrochloric acid (12 mol/L) was refluxed for about 2 h to separate out a white solid, which was recrystallized with ethanol to produce white crystals of 2-bromo-spirofluorene (1.2 g, yield 63%).
GC-MS (m/z +): 394. 1HNMR (400 MHz, CDCl3, ppm):δ7.80～7.86 (m, 3H), δ7. 70 (d, 1H),δ7.48 (m, 1H), δ7.36 ～ 7.40 (m, 3H), δ7.13 (m, 3H), δ6.84 (d, 1H), δ6.72 (m, 3H)

9-([1,1'-biphenyl]-2-yl)-2-bromo-9H-fluoren-9-ol

236389-20-1
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171408-76-7
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Yield:171408-76-7 97%

Reaction Conditions:

with acetic acid;sulfuric acid for 1 h;Heating;

Steps:

7

Preparation of Structural Formula 48B; Structural Formula 48A (27.3 g, 66.1 mmol) was added to 200 ml of glacial acetic acid, and heated, and 0.1 ml of sulfuric acid was added thereto, and heated and agitated for 1 hour. The solid that was generated after the temperature was lowered to normal temperature was filtered, washed with 300 ml of water, and 100 ml of ethanol, and dried to obtain Structural Formula 48B (25.4 g, yield 97%). MS: [M+H]⁺= 396

References:

EP2343277,2011,A2 Location in patent:Page/Page column 44-45

3096-56-8 Synthesis