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Synthesis method of cyclic sulfate

A technology of cyclic sulfate and cyclic sulfite, which is applied in the field of preparation of cyclic sulfate, can solve the problems of cumbersome catalyst recovery, expensive catalyst, and a lot of waste water, and achieve the effect of low cost, low price and simple separation

Pending Publication Date: 2022-03-15
HUNAN ASTAR BIO CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Benefits of technology

This patented technology has several benefits: it're gentle at reacting with other chemical agents, easy-to-use equipment for treatments like acidification, reducing costs by utilizing cheap materials such as Fe2O3 instead of expensive raw material (iron). It also produces very pure products from reduced amounts of waste generated during production processes without any harmful impurities.

Problems solved by technology

This patented technical problem addressed in this patents relates to finding better ways to produce more pure chemical substances that have improved characteristics such as lower resistance at higher temperatures than current materials while also being cost-effective compared to previous processes.

Method used

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  • Synthesis method of cyclic sulfate
  • Synthesis method of cyclic sulfate
  • Synthesis method of cyclic sulfate

Examples

Experimental program
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Embodiment 1

[0019] Under oxygen atmosphere (20L oxygen bag, normal pressure), add Fe(NO 3 ) 3 9H 2 O (406mg, 1mmol), 4-OH-TEMPO (342mg, 2mmol), NaCl (118mg, 2mmol), pentaerythritol bicyclic sulfite (2.28g, 10mmol), 40ml of dichloroethane solvent, stirred the reaction at 50°C 12 hours to end the reaction, transfer to a separatory funnel, add 50 ml of water, fully wash, the organic phase is dried with anhydrous sodium sulfate and distilled under reduced pressure to recover dichloroethane, and the residue is subjected to silica gel column chromatography, ethyl acetate and petroleum Ether was used as the mobile phase, the solvent was removed, and vacuum-dried to obtain 2.34 g of pentaerythritol bicyclic sulfate as a white solid, with a yield of 90% and a gas-phase purity of 99%. 1 H NMR (400MHz, CD 3 COCD 3 )δ5.02(s,8H).

Embodiment 2

[0021] Add Fe(NO 3 ) 3 9H 2 O (8g, 20mmol), 4-OH-TEMPO (6.84g, 40mmol), NaCl (2.36g, 40mmol), 32.4 grams of vinyl sulfite (0.3 moles), 900 milliliters of dichloroethane solvent, at 100ml / min Continue to feed air at a constant flow rate, stir and react at 30°C for 6 hours to end the reaction, transfer to a separatory funnel, add 1000 ml of water, wash thoroughly, dry the organic phase with anhydrous sodium sulfate, and distill under reduced pressure to recover dichloroethane, and the remaining The product was vacuum-dried to obtain a crude vinyl sulfate product, which was recrystallized with dichloromethane to obtain 26 g of white crystalline vinyl sulfate, with a yield of 70%, a melting range of 98-99° C., and a gas-phase purity of 99%.

Embodiment 3

[0023] In the autoclave, 4-methyl vinyl sulfite (0.3 mol) was dissolved in 900 ml of toluene, kept at 45 ° C, and iron sulfate (20 mmol), TEMPO (40 mmol), NaCl (2.36 g, 40 mmol) were added successively under stirring, In an oxygen atmosphere of 5 atmospheres, stir and react for 10 hours, separate the organic phase and dry it with anhydrous sodium sulfate, and carry out vacuum distillation (50°C / 1mmHg) after the filtrate is precipitated to obtain 29.8 grams of transparent liquid 4-methyl Vinyl sulfate, yield 72%, gas phase purity 99%.

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Abstract

The invention belongs to the technical field of organic synthetic chemistry, and particularly relates to a preparation method of cyclic sulfate, under the action of a catalyst and in the presence of oxygen or air, cyclic sulfite is subjected to an oxidation reaction to obtain the cyclic sulfate, the catalyst is a mixture of ferric salt, chlorate and tetramethylpiperidine oxide, the ferric salt is ferric nitrate, ferric sulfate, ferric chloride, ferric phosphate or the ferric salt with crystal water, the chlorate is sodium chloride or potassium chloride, and the tetramethylpiperidine oxide is 2, 2, 6, 6-tetramethylpiperidine oxide or 4-hydroxy-2, 2, 6, 6-tetramethylpiperidine oxide; the method is efficient, low in cost and green in synthesis of the cyclic sulfate.

Description

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Claims

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Application Information

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Owner HUNAN ASTAR BIO CHEM TECH
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