POTASSIUM 4-BROMOPHENYLTRIFLUOROBORATE synthesis
- Product Name:POTASSIUM 4-BROMOPHENYLTRIFLUOROBORATE
- CAS Number:374564-35-9
- Molecular formula:C6H4BBrF3K
- Molecular Weight:262.9
5467-74-3
374564-35-9
GENERAL STEPS: In a reaction vessel equipped with a charging funnel, 4-bromophenylboronic acid (5 mmol) was dissolved in methanol (10 mL). A solution of potassium hydrogen fluoride (KHF2, 1.56 g, 20 mmol) in water (8 mL) was added slowly and dropwise. The reaction mixture was stirred at room temperature for 30 min. Subsequently, the mixture was concentrated under high vacuum to remove the solvent. The residual solid was extracted with an acetone solution of 20% methanol (4 x 10 mL). The extracts were combined, concentrated to near saturation, and then ether (Et2O) was added until no further precipitate was produced. The precipitate was collected by filtration, washed with ether (2 × 10 mL), and finally dried under high vacuum to give a potassium 4-bromophenyl trifluoroborate product of sufficient purity for subsequent characterization.
5467-74-3
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374564-35-9
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Yield:374564-35-9 87%
Reaction Conditions:
with potassium hydrogenfluoride in methanol;water at 0; for 0.5 h;
Steps:
2.1 General Procedure for Preparation of Potassium Organotrifluoroborates (2a-j)
General procedure: To a solution of the appropriate boronic acid, 1a-j (5 mmol) in MeOH (10 mL) was added dropwise a solution of KHF2 (1.56 g, 20 mmol) in H2O (8 mL) using an addition funnel. The mixture was stirred for 30 min and concentrated under high vacuum. The residual solid was extracted with four portions of 20% MeOH in acetone. The combined extracts were concentrated close to the saturation point and Et2O was added until no more precipitation was observed. The solid was collected, washed with two portions of Et2O, and dried under high vacuum to give the corresponding products sufficiently pure for characterization.
References:
Liesen, André P.;Silva, Arisson T.;Sousa, Jokderléa C.;Menezes, Paulo H.;Oliveira, Roberta A. [Tetrahedron Letters,2012,vol. 53,# 32,p. 4240 - 4242] Location in patent:supporting information; experimental part
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374564-35-9
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5467-74-3
473 suppliers
$8.00/1g
374564-35-9
97 suppliers
$7.00/250mg