ChemicalBook CAS DataBase List 18-Crown-6

18-Crown-6 synthesis

12synthesis methods

Product Name:18-Crown-6
CAS Number:17455-13-9
Molecular formula:C12H24O6
Molecular Weight:264.32

112-27-6 Synthesis

112-27-6
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17455-13-9
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$5.00/10g

Yield:17455-13-9 65.2%

Reaction Conditions:

with 4-methylbenzene-1-sulfonyl chloride;potassium hydroxide in tetrahydrofuran at 55 - 60; for 3 h;

Steps:

1-3 Example 2

A preparation method of 18-crown-6, the production steps are as follows:(1) Weigh 15g of triethylene glycol and 12g of potassium hydroxide into a 500mL reaction bottle, then add 300mL of tetrahydrofuran to the reaction bottle, and start stirring;(2) Add 19g of p-toluenesulfonyl chloride dropwise to the reaction bottle, control the reaction temperature at 55-60 , and react for 3h;(3) Add 7.7g of diethyl sulfate to the solution after the reaction to separate potassium p-toluenesulfonate, control the reaction temperature at 80 ° C, and react for 3h to produce diethyl p-toluenesulfonate and potassium sulfate;(4) The final solution obtained after the reaction is filtered, concentrated, and vacuum distilled, and the distillate contains 18-crown-6, diethyl p-toluenesulfonate, triethylene glycol, etc .;(5) After washing the distillate with 20 mL of distilled water and leaving it to separate into layers, the upper layer solution is diethyl p-toluenesulfonate, the lower layer solution is 18-crown-6, triethylene glycol, etc. The lower layer solution is centrifugally separated Precipitation, the precipitate is dried to obtain 18-crown-6.The mass of 18-crown-6 finally prepared was 17.2 g, and the yield was 65.2%.

References:

CN110759886,2020,A Location in patent:Paragraph 0022-0045

112-26-5 Synthesis