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ChemicalBook CAS DataBase List Sulfolane

Sulfolane synthesis

10synthesis methods
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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

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