TETRABUTYLAMMONIUM METHANESULFONATE synthesis
- Product Name:TETRABUTYLAMMONIUM METHANESULFONATE
- CAS Number:65411-49-6
- Molecular formula:C17H39NO3S
- Molecular Weight:337.56
616-42-2
188 suppliers
$12.00/5g
1643-19-2
980 suppliers
$12.00/10g
65411-49-6
31 suppliers
$129.00/10g
Yield:65411-49-6 100%
Reaction Conditions:
at 110 - 115; under 750.075 - 1125.11 Torr; for 96 h;Product distribution / selectivity;
Steps:
9
Example 9 Tetrabutylammonium Methanesulfonate A mixture of 12.94 g (40.14 mmol) of tetrabutylammonium bromide and 5.15 g (46.76 mmol) of dimethyl sulfite is stirred at 110-115° C. (temperature of the oil bath) for 96 hours under an inert-gas atmosphere (nitrogen) in a sealed reaction vessel with pressure valve for 1-1.5 bar above atmospheric pressure. The end of the reaction is determined by NMR measurement. The product is pumped off over the course of 5 hours in vacuo at 13.3 Pa and 115° C. (temperature of the oil bath), giving 13.53 g of tetrabutylammonium methanesulfonate as a solid. The melting point is 83-84° C. The yield is virtually quantitative. The residual bromide content is less than 5 ppm. The product is investigated by means of NMR spectroscopy. 1H NMR (reference: TMS; solvent: CD3CN), ppm: 0.95 t (CH3); 1.34 t,q (CH2); 1.60 m (CH2); 2.39 s (CH3); 3.11 m (CH2); 3JH,H=7.4 Hz. Elemental analysis: found, %: C, 60.47; H, 11.90; N, 4.18; S, 9.60; calculated for C17H39NO3S, %: C, 60.49; H, 11.65; N, 4.15; S, 9.50.
References:
US2008/221334,2008,A1 Location in patent:Page/Page column 10
75-75-2
604 suppliers
$10.00/5g
1643-19-2
980 suppliers
$12.00/10g
65411-49-6
31 suppliers
$129.00/10g
616-42-2
188 suppliers
$12.00/5g
10534-59-5
288 suppliers
$5.00/5g
65411-49-6
31 suppliers
$129.00/10g