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Chemical Structure| 1211547-22-6 Chemical Structure| 1211547-22-6

Structure of 1211547-22-6

Chemical Structure| 1211547-22-6

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Product Details of [ 1211547-22-6 ]

CAS No. :1211547-22-6
Formula : C25H16Br2
M.W : 476.20
SMILES Code : BrC1=CC=CC(=C1)C1(C2C=CC=C(C=2)Br)C2=CC=CC=C2C2=CC=CC=C12
MDL No. :MFCD32709914

Safety of [ 1211547-22-6 ]

GHS Pictogram:
Signal Word:Warning
Hazard Statements:H302-H315-H319
Precautionary Statements:P501-P270-P264-P280-P302+P352-P337+P313-P305+P351+P338-P362+P364-P332+P313-P301+P312+P330

Application In Synthesis of [ 1211547-22-6 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 1211547-22-6 ]

[ 1211547-22-6 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 110-71-4 ]
  • [ 2052-07-5 ]
  • [ 25032-74-0 ]
  • [ 106-93-4 ]
  • [ 1211547-22-6 ]
YieldReaction ConditionsOperation in experiment
With hydrogen bromide; magnesium; In tetrahydrofuran; acetic acid; toluene; A) 9,9-Bis(3-bromophenyl)-9H-fluorene 62.9 g (270 mmol) of 2-bromobiphenyl mixed with 400 ml of THF, 550 ml of toluene, 45 ml of 1,2-dimethoxyethane and 2.6 ml of 1,2-dibromoethane are reacted with 6.6 g (250 mmol) of magnesium to give the corresponding Grignard compound. A solution of 60.0 g (176 mmol) of bis(3-bromophenyl) ketone in 600 ml of THF is added dropwise to the cooled Grignard solution. When the addition is complete, the reaction mixture is heated under reflux for 4 h, the solvent is then removed in vacuo, the residue is dissolved in 700 ml of glacial acetic acid, 10 ml of hydrogen bromide in 30% glacial acetic acid are added, and the mixture is heated under reflux for 6 h. After cooling with stirring, the precipitated solid is filtered off with suction, washed twice with 200 ml of glacial acetic acid each time and three times with 300 ml of ethanol each time and then dried in vacuo. Yield: 69.0 g (145 mmol), 82.1%, 99% pure according to 1H-NMR.
  • 2
  • [ 2052-07-5 ]
  • [ 25032-74-0 ]
  • [ 1211547-22-6 ]
YieldReaction ConditionsOperation in experiment
92% Firstly, magnesiums (6.73 g, 255.8 mmol) areintroduced to the flask including one iodine crystal. 2- bromo biphenyls (64.4g, 276.3 mmol), the anhydrous tetrahydrofuran of 400 ml, the anhydrous tolueneof 500 ml, and 1,2- dimethoxyethane of 45 ml and 1,2- dichloroethane of 2.65 mlare introduced within the dropping funnel. The outbound - material blend isdipped as the gradually. The reactant is cooled under the reflux for theadditional 1 hour after doing the mixing. Bis - (3- bromo-phenyl) methanones(61.4 g, 180.6 mmol) are dissolved among THF of 600 ml and it dips as thegradually. The reactant is stirred under the reflux for 5 hours. Thearrangement is filtered and THF is evaporated in the Rotavapor. The acetic acidof 500 ml, and the acetic acid of 200 ml and HBr of 10 ml are added and themixture is stirred under the reflux for 64 hours. The solid in which the colouris pale is filtered to the suction and it washes to the ethyl acetate andethanol. The yield is 79.8 g (92% of the Theoretical value) as the white solid
91% About 10 ml of a solution of 2-bromobiphenyl (80.0 g, 343 mmol) and 1,2-dibromoethane (3.6 ml, 43 mmol) in a mixture of 640 ml of toluene, 520 mlof tetrahydrofuran and 60 ml of ethylene glycol dimethyl ether are added to8.8 g of magnesium (334 mmol) and heated. After onset of the reaction,the heating is removed and the remaining solution is added dropwise insuch a way that reflux is maintained. On completion of addition, the mixtureis heated to reflux for 1 h. Subsequently, under gentle reflux, a solution ofthe ketone KI (80.0 g, 235 mmol) in 800 ml of tetrahydrofuran is addeddropwise and the mixture is stirred under reflux for 5 h. The heating isremoved and the mixture is stirred for 14 h. The solvents are removedcompletely on a rotary evapourator. The remaining residue is taken up in amixture of 920 ml of glacial acetic acid and 13.2 ml of a 33% solution of hydrogen bromide in acetic acid, and heated to reflux for 6 h. After removing the heating, the mixture is stirred for 16 h. The solid material formed is filtered off with suction, washed with about 150 ml of glacial acetic acid and three times with 250 ml each time of ethanol and then dried in a vacuum drying cabinet. This leaves 101.6 g (213 mmol, 91% of theory)of the product as a light grey solid having a purity of about 99% by 1 HNMR.
82.1% 62.9 g (270 mmol) of 2-bromobiphenyl mixed with 400 ml of THF, 550 ml of toluene, 45 ml of 1,2-dimethoxyethane and 2.6 ml of 1,2-dibromoethane are reacted with 6.6 g (250 mmol) of magnesium to give the corresponding Grignard compound. A solution of 60.0 g (176 mmol) of bis(3-bromophenyl) ketone in 600 ml of THF is added dropwise to the cooled Grignard solution. When the addition is complete, the reaction mixture is heated under reflux for 4 h, the solvent is then removed in vacuo, the residue is dissolved in 700 ml of glacial acetic acid, 10 ml of hydrogen bromide in 30% glacial acetic acid are added, and the mixture is heated under reflux for 6 h. After cooling with stirring, the precipitated solid is filtered off with suction, washed twice with 200 ml of glacial acetic acid each time and three times with 300 ml of ethanol each time and then dried in vacuo. Yield: 69.0 g (145 mmol), 82.1%, 99% pure according to1H-NMR.
 

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