Glycol sulfite synthesis
- Product Name:Glycol sulfite
- CAS Number:3741-38-6
- Molecular formula:C2H4O3S
- Molecular Weight:108.12
107-21-1
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3741-38-6
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$6.00/5g
Yield:3741-38-6 99%
Reaction Conditions:
Stage #1:ethylene glycol with thionyl chloride in dichloromethane at 0 - 20; for 2 h;
Stage #2: with triethylamine in dichloromethane for 1 h;Time;
Steps:
1 Example 1
In a 0.5 L reactor, 40 g (0.644 mol) of ethylene glycol was added.220ml of dichloromethane as a solvent,The temperature of the reaction kettle was controlled to be 0-5 ° C, and 92 g (0.773 mol) of thionyl chloride was slowly added dropwise.After the completion of the dropwise addition, the mixture was kept at room temperature for 2 hours, and then 78.2 g (0.773 mol) was added dropwise to the reaction vessel.Triethylamine was continued for 1 h after the addition was completed. The reaction system was taken out and suction filtered.The obtained precipitate was triethylamine hydrochloride, and the filtrate was subjected to distillation under reduced pressure to recover dichloromethane.The remainder is vinyl sulfite,Obtaining 68.98 g of ethylene sulfite (yield 99%), the purity of the GC detection is 99.1%; 20 g of the obtained vinyl sulfite and 44.81 g of dibenzoyl peroxide were added together to 200 ml of dichloromethane, and then 0.1 g of pyridine chlorochromate was added thereto, and reacted at room temperature for 6 hours, and the solvent and the low-boiling point were distilled off under reduced pressure. The product was obtained and the obtained solid was recrystallized from dichloromethane.Obtained white crystals 20.43 g, yield 89%,The purity of the detected vinyl acetate was 99.6%, and the water content was ≤20 ppm.
References:
Shandong Yonghao New Materials Technology Co., Ltd.;Niu Huizhu CN109516971, 2019, A Location in patent:Paragraph 0016; 0017; 0018; 0019; 0020; 0021
616-42-2
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107-21-1
1294 suppliers
$10.00/25g
3741-38-6
241 suppliers
$6.00/5g
75-21-8
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3741-38-6
241 suppliers
$6.00/5g
107-21-1
1294 suppliers
$10.00/25g
3741-38-6
241 suppliers
$6.00/5g
107-06-2
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