![](/CAS/20150408/GIF/1361227-58-8.gif)
3-DroMo-9,9'-spirobifluorene synthesis
- Product Name:3-DroMo-9,9'-spirobifluorene
- CAS Number:1361227-58-8
- Molecular formula:C25H15Br
- Molecular Weight:395.29
![2-Bromobiphenyl](/CAS/GIF/2052-07-5.gif)
2052-07-5
385 suppliers
$16.30/1g
![3-Bromo-9H-fluoren-9-one](/CAS/GIF/2041-19-2.gif)
2041-19-2
108 suppliers
$16.00/250mg
![3-DroMo-9,9'-spirobifluorene](/CAS/20150408/GIF/1361227-58-8.gif)
1361227-58-8
97 suppliers
$18.00/100mg
Yield:1361227-58-8 94%
Reaction Conditions:
Stage #1:2-Bromobiphenyl with n-butyllithium in diethyl ether at -60;
Stage #2:3-bromofluoren-9-one in diethyl ether at 45;
Stage #3: with hydrogenchloride;acetic acid in 1,4-dioxane
Steps:
1.2 3-bromo-SBF
[0090] This compound was made in two steps from 3-bromofluorenone obtained in step 1. First, 2-bromobiphenyl (1.05 equivalents, 4.0 g, 16.5 mmol) is solubilised in 102 ml of anhydrous diethyl ether. This solution is cooled to -60°C and n-BuLi (1.16 eq.) is added dropwise. After 10 min at this temperature, a white precipitate appeared which was redissolved while the medium was warmed to room temperature. 3-Bromofluorenone was then added and the reaction mixture was kept at 45 °C for one night. [0091] After addition of NH4Cl (5% aq., 260 ml) and extraction with diethyl ether, 7.0 g of an alcohol was obtained. This solid was solubilised in 141 ml of acetic acid and hydrolyzed by the addition of 78 ml of HCl/dioxane (10 % mol., 20 eq.). After evaporation of the solvents, the solid was subjected to normal phase flash chromatography to afford 5.86 g of the target compound (94 % yield).
References:
SOLVAY SA;The designation of the inventor has not yet been filed EP2574608, 2013, A1 Location in patent:Paragraph 0088; 0089; 0090; 0091
![3-Bromo-9H-fluoren-9-one](/CAS/GIF/2041-19-2.gif)
2041-19-2
108 suppliers
$16.00/250mg
![Lithium, [1,1'-biphenyl]-2-yl-](/CAS/20200119/GIF/55365-18-9.gif)
55365-18-9
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![3-DroMo-9,9'-spirobifluorene](/CAS/20150408/GIF/1361227-58-8.gif)
1361227-58-8
97 suppliers
$18.00/100mg
![3-Bromo-9H-fluoren-9-one](/CAS/GIF/2041-19-2.gif)
2041-19-2
108 suppliers
$16.00/250mg
![2-BIPHENYLYLMAGNESIUM BROMIDE 0.5M IN](/CAS/GIF/82214-69-5.gif)
82214-69-5
22 suppliers
$255.00/50mL
![3-DroMo-9,9'-spirobifluorene](/CAS/20150408/GIF/1361227-58-8.gif)
1361227-58-8
97 suppliers
$18.00/100mg
![3-Bromo-9H-fluoren-9-one](/CAS/GIF/2041-19-2.gif)
2041-19-2
108 suppliers
$16.00/250mg
![2-Iodobiphenyl](/CAS/GIF/2113-51-1.gif)
2113-51-1
259 suppliers
$6.00/1g
![3-DroMo-9,9'-spirobifluorene](/CAS/20150408/GIF/1361227-58-8.gif)
1361227-58-8
97 suppliers
$18.00/100mg
![2-Amino-4'-bromobenzophenone](/CAS/GIF/135776-98-6.gif)
135776-98-6
76 suppliers
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![3-DroMo-9,9'-spirobifluorene](/CAS/20150408/GIF/1361227-58-8.gif)
1361227-58-8
97 suppliers
$18.00/100mg