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2401-22-1

1-chloro-2-iodo-4-methyl-benzene synthesis

4synthesis methods
-

Yield:2401-22-1 92.1%

Reaction Conditions:

with sulfuryl dichloride;diphenyl sulfide;antimony(III) chloride in 1,2-dichloro-ethane at 20 - 25; for 6 h;

Steps:

12 [Example 12]

1 g of m-iodotoluene (4.59 mmol; manufactured by Manac),0.021 g (0.09 mmol; manufactured by Wako Pure Chemical Industries, Ltd.) of antimony chloride (III) and 0.017 g (0.09 mmol, diphenyl sulfide manufactured by Wako Pure Chemical Industries, Ltd.) were dissolved in 5 g of ethylene dichloride,Subsequently, 0.74 g (5.5 mmol; manufactured by Wako Pure Chemical Industries, Ltd.) of sulfuryl chloride was added,The reaction was carried out at 20 to 25 ° C. for 6 hours. After completion of the reaction,A 10 wt% hydrochloric acid aqueous solution was added,After stirring for a while,The organic layer was separated.Then,Neutralized with a 10 wt% aqueous sodium hydroxide solution,The organic layer was separated.The purity of the target product and the by-product content in the obtained reaction solution were measured by GC.Monochloro-3-iodotoluene: 92.10%, halosubstituted product (by-productThing): 0.10%.

References:

JP6074279,2017,B2 Location in patent:Paragraph 0048