NMR data for tris(1,1,1,3,3,3-hexafluoro-2-(trifluoromethyl)propan-2-yl) borate

DOI: 10.14469/hpc/14833 Metadata

Created: 2024-11-09 08:52

Last modified: 2024-11-15 13:49

Author: Henry Rzepa

License: Creative Commons: Public Domain Dedication 1.0

Funding: (none given)

Description

Under an atmosphere of argon, a flame dried 2-necked round bottom flask equipped with a condenser was charged with perfluoro-tert-butanol (7.5 ml, 12.75g, 54 mmol, 3.15 eq.) and cooled to 0 °C. Borane dimethylsulfide (1.7 ml, 17 mmol, 1 eq) was added dropwise, and after 30 minutes the cold bath was removed and the reaction heated to reflux overnight. After this time 1 ml further perfluoro-tert-butanol was added and reflux was continued for 2 hours. After this time the borate was purified by distillation (100 °C, 40 mbar) and collected as a white solid. The solid was melted by gentle heating and solid impurities were removed by filtration. Yield = 5.75 g colourless liquid, 47%. Due to poor solubility in typical NMR solvents, analysis was carried out in anhydrous diethyl ether. NMR data is in accordance with literature reports.

Member of collection / collaboration

DOIDescription
10.14469/hpc/14865 NMR Data for Borate Catalysts

Members

DOIDescription
10.14469/hpc/14834 NMR data for tris(1,1,1,3,3,3-hexafluoro-2-(trifluoromethyl)propan-2-yl) borate. 13C
10.14469/hpc/14835 NMR data for tris(1,1,1,3,3,3-hexafluoro-2-(trifluoromethyl)propan-2-yl) borate. 11B
10.14469/hpc/14836 NMR data for tris(1,1,1,3,3,3-hexafluoro-2-(trifluoromethyl)propan-2-yl) borate. 19F

Associated DOIs

Current dataset ...DOIDescription
References 10.1002/chem.201104055 Direct Amide Coupling of Non-activated Carboxylic Acids and Amines Catalysed by Zirconium(IV) Chloride

Subject Keywords

KeywordValue
Inchi InChI=1S/C12BF27O3/c14-4(15,16)1(5(17,18)19,6(20,21)22)41-13(42-2(7(23,24)25,8(26,27)28)9(29,30)31)43-3(10(32,33)34,11(35,36)37)12(38,39)40
Inchikey ZWTOJDDJAARGAE-UHFFFAOYSA-N

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