Sulfolane synthesis
- Product Name:Sulfolane
- CAS Number:126-33-0
- Molecular formula:C4H8O2S
- Molecular Weight:120.17
110-01-0
126-33-0
GENERAL METHOD: To a well-stirred solution of tetrahydrothiophene (1 mmol) and diethylamine (0.2 mmol) in acetonitrile (2 mL) was slowly added a solution of Oxone (1.5 mmol) in water (4 mL). The reaction mixture was stirred continuously at room temperature and the progress of the reaction was monitored by thin layer chromatography (TLC). Upon completion of the reaction, the mixture was diluted with ice water. If the product, cyclobutanesulfone, was solid, it was separated directly by simple filtration; if the product was liquid, it was extracted with ethyl acetate. The organic phase was washed sequentially with water, dried over anhydrous sodium sulfate and subsequently concentrated under reduced pressure to remove the solvent. The residue was purified by short silica gel column chromatography to give pure cyclobutanesulfone.
26978-64-3
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126-33-0
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$5.00/25g
Yield:126-33-0 113.5 g
Reaction Conditions:
with acetic acid in water at 135 - 155; under 1 - 3 Torr; for 0.8 h;Temperature;
Steps:
1; 2; 3 Preparation of 1,4-butane sultone
To the reaction flask, 142 g of the above-mentioned intermediate chlorobutyl acetate, 220 g of sodium sulfite, and water were added to a saturated solution of sodium sulfite.Install a reflux device, stir and heat to reflux, time 15h, the solution becomes clear, the reaction is finished, and some water is recovered under reduced pressure until solids are precipitated.Cool down to below 45 ° C, add methanolic hydrochloric acid (41.9%, to pH 3), stir for 1.5 h,Cooling to 6 ° C, suction filtration, the filter cake is a by-product salt of sodium chloride, the filtrate is first decompressed to produce methanol water and acetic acid,The oil bath was raised to 135 ° C high vacuum decompression and entanglement for 0.8 h, the oil bath was heated to 155 ° C, 1-3 mmHg high vacuum decompression production products,Obtained a colorless transparent liquid of 113.5g,That is, 1,4-butane sultone, the yield was 88.49%.
References:
CN109776484,2019,A Location in patent:Paragraph 0010; 0030; 0033-0034; 0036; 0039-0040; 0042-0046
110-01-0
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126-33-0
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77-79-2
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126-33-0
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110-01-0
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1600-44-8
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126-33-0
531 suppliers
$5.00/25g
1600-44-8
135 suppliers
$37.70/10g
126-33-0
531 suppliers
$5.00/25g