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ChemicalBook CAS DataBase List 1,4-Dichlorobutane

1,4-Dichlorobutane synthesis

13synthesis methods
-

Yield:110-56-5 97%

Reaction Conditions:

with hydrogenchloride;ammonium chloride in water at 56 - 105; for 3 h;

Steps:

3 Example 3 The preparation method of 1,4-dichlorobutane, the steps as follows:

Into a 1000ml reaction flask with oil-water separator and condenser,Put in 400 grams of water, 5 grams of ammonium chloride, and 322 grams of 1,4-butanediol in sequence, and stir and raise the temperature to 56°C;Start to pass HCL gas. When the clear and transparent reaction liquid in the reaction flask becomes milky white, continue to pass HCL gas, increase the temperature of the reaction liquid to 105°C, and start reflux and liquid separation;As the reflux reaction progresses, there is stratification in the oil-water separator. The reflux reaction is 3 hours, and the molar ratio of 1,4-butanediol to HCL gas is 1:2.6;The lower water phase is refluxed into the reaction flask, and the upper oil layer is 1,4-dichlorobutane separated and collected.The purity determined by HPLC was 99.5%, and the yield based on 1,4-dichlorobutane was 97%.

References:

CN112341309,2021,A Location in patent:Paragraph 0020

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