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ChemicalBook CAS DataBase List 1-Bromooctane

1-Bromooctane synthesis

15synthesis methods
1-Bromooctane is prepared by reacting octanol with hydrobromic acid. After the sodium bromide was completely dissolved with sulfuric acid, n-octanol was added, heated to reflux for 7-8 hours, cooled and diluted with water, the organic phase was separated, washed with water, concentrated sulfuric acid, water, and 10% sodium carbonate solution in turn, and washed with anhydrous sulfuric acid. Sodium dry. Distillation of 196-200°C, or 91-93°C (2.93kPa) fraction, is the finished product of 1-bromooctane. The yield is over 90%.
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Yield:111-83-1 98%

Reaction Conditions:

with sulfuric acid;hydrogen bromide in lithium hydroxide monohydrate at 60;Flow reactor;Green chemistry;Temperature;

Steps:

1.1; 1.2; 1.3; 1.4; 1.5; 2.1; 2.2; 2.3; 2.4; 2.5; 3.1; 3.2; 3.3; 3.4; 3.5

(1) The molar ratio of n-octanol to hydrobromic acid is 1: 1.1, that is, take 41.2g of n-octanol and 70g of 40% hydrobromic acid into two containers;(2) The molar ratio of n-octanol to concentrated sulfuric acid is 1: 0.8, that is, take 26g of concentrated sulfuric acid and hydrobromic acid and mix them in the microreactor;(3) Use a constant flow pump to pump concentrated sulfuric acid and hydrobromic acid into the microreactor, and then pump n-octanol to control the flow rate of the pumped solution to 0.4 mL / min;(4) maintaining the reaction temperature at 60 ° C;(5) Dilute the collected solution with water, separate the organic layer, and obtain a 1-bromo-n-octane yield of 98% after purification.

References:

CN110655445,2020,A Location in patent:Paragraph 0017-0037

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