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ChemicalBook CAS DataBase List 1-Chlorobutane

1-Chlorobutane synthesis

11synthesis methods
1-Chlorobutane is obtained by esterification of n-butanol with hydrogen chloride or hydrochloric acid at 100℃ either without a catalyst or utilizing the accelerating effect of zinc chloride, tripentylamine hydrochloride, or phosphorus pentachloride. n-Butyl chloride is also obtained, along with 2-chlorobutane, by the chlorination of butane over aluminum oxide at 200℃.
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Yield:109-69-3 96.9%

Reaction Conditions:

with hydrogenchloride in water at 115; for 2 h;Reagent/catalyst;Temperature;

Steps:

1-6 Example 5

Add 300ml of 2,3,5,6-tetramethyldioxane, 20ml of purified water and 200ml (2.19mol) of n-butanol to a three-necked flask with a capacity of 1000ml equipped with a stirrer and a thermometer. Stir and raise the temperature to 115 , 196.4g (5.38mol) of hydrogen chloride gas is introduced, and the reaction is distilled. As the reaction time increases, fractions are gradually distilled out. After 100ml of fractions are distilled out, use a peristaltic pump to feed the reaction flask at a rate of 3ml/min. Add n-butanol, add 800ml (8.74mol) of n-butanol in total, keep the hydrogen chloride gas at a 3g/min feed rate during the addition, and after completing the heat preservation distillation and reaction for 2h, Almost no fraction is distilled out further. The reaction is over. After the obtained fractions are layered, the upper organic layer is 1-chlorobutane. The final 1-chlorobutane is 980.6g (10.59mol), the molar yield is 96.9%, and the GC purity 99.89%.

References:

CN112707789,2021,A Location in patent:Paragraph 0039-0058

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