1-Bromo-2-methylpropane synthesis

13synthesis methods

Product Name:1-Bromo-2-methylpropane
CAS Number:78-77-3
Molecular formula:C4H9Br
Molecular Weight:137.02

78-83-1 Synthesis

78-83-1
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78-77-3
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Yield:78-77-3 42.9%

Reaction Conditions:

with sulfuric acid;hydrogen bromide in water at 90 - 95;

Steps:

6 Comparative Example 6. Synthesis of bromoisobutane

Add 300 g (4.047 mol) of isobutanol to the reaction flask, 1800 g (10.679 mol) of 48% hydrobromic acid, and then slowly drop 400 g (4.079 mol) of sulfuric acid.Heating to 90 95 , holding reaction for 12 16hr; changing reflux to distillation,The temperature was further increased to 100-140 ° C in stages, and the distillate was collected (adding an appropriate amount of water according to the actual situation during the distillation process), until essentially no oil was distilled off, standing still, and separating the oil layer; adding methylene chloride to the aqueous phase 600g, stirred for extraction, separated the dichloromethane layer; combined the oil layer and the dichloromethane layer, washed twice with a 5% sodium bicarbonate aqueous solution, separated the organic phase, and concentrated the dichloromethane at normal pressure to obtain a crude bromoisobutane About 435g, GC detection, purity about 78%,Among them, bromine tert-butane is about 12%, isobutanol is about 5%, and bromo-sec-butane is about 0.8%.Bromo-n-butane was about 0.3%; the obtained crude product was rectified through a Kirschner column, and a fraction of 92 to 95 ° C was collected to obtain about 238 g of bromo-isobutane (theoretical amount: 554.6 g). The yield was 42.9%. GC detection,The purity is about 99.2%, of which about 0.28% is bromo-t-butane and about 0.23% is bro-secBromo-n-butane is about 0.14%.

References:

CN110790720,2020,A Location in patent:Paragraph 0098-0100

75-28-5 Synthesis