ChemicalBook CAS DataBase List Fluorotributyltin

Fluorotributyltin synthesis

3synthesis methods

Product Name:Fluorotributyltin
CAS Number:1983-10-4
Molecular formula:C12H27FSn
Molecular Weight:309.05

960-16-7
95 suppliers
$22.60/1g

13400-13-0 Synthesis

13400-13-0
251 suppliers
$10.00/5g

1983-10-4
50 suppliers
$30.89/5g

Yield:1983-10-4 87%

Reaction Conditions:

with bis-triphenylphosphine-palladium(II) chloride;copper(l) iodide;bromobenzene;lithium chloride in N,N-dimethyl-formamide at 110; for 12 h;Inert atmosphere;Reagent/catalyst;

Steps:

1
Second, A mixture of 1.58 g (10 mmol) of bromobenzene, 3.864 g (10.5 mmol) of tributylphenyltin, 0.163 g (0.85 mmol) of cuprous iodide, 1.275 g (30 mmol) of lithium chloride, 283 mg (0.4 mmol ) triphenylphosphine palladium dichloride, 3.042 g (20 mmol) of cesium fluoride dissolved in 50 ml of DMF (N, N-dimethylformamide) was added to a three-necked flask, nitrogen was replaced three times, reacted at 110 ° C for 12 h. The solution was thoroughly purified by thin layer chromatography (TLC). after cooling to room temperature, 30 mL of saturated potassium fluoride solution was added and stirred for 15 min. The filtrate was collected by filtration and the filtrate was extracted with n-hexane. The organic layer was dried over anhydrous sodium sulfate and the filtrate was steamed to obtain a pale yellow solid which was separated by column (stationary phase: silica gel, mobile phase: n-hexane) and evaporated to dryness to give 1.483 g of colorless crystalline biphenyl (yield: 97%) , Melting point : 68.2 to 68.7 ° C, wherein the concentration of cesium fluoride in the mixed solution is 0.4 mol / L. Third, the residue obtained in step 2 at 0.05atm, 56 for vacuum drying 8h, cooled to room temperature, 3.512g vacuum drying after the residue with 35ml acetone ultrasonic solution, after standing for 1h after filtration, the filter was insoluble, the filtrate was concentrated by centrifugation in 140 mL of absolute ethanol and the filtrate was concentrated by spin steam and dried to give 2.823 g of a white powder of tributyltin fluoride (yield: 87%), melting point: 270.5 to 271.3 ° C.

References:

QIQIHAR UNIVERSITY;SONG, WEIMING;SUN, LI;BAI, WEIWEI;LI, SHIXING;DENG, QIGANG CN105016961, 2016, B Location in patent:Paragraph 0051; 0053-0054

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